#------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/55/7035521.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7035521
loop_
_publ_author_name
'Du, Xia'
'Li, Zijian'
'Liu, Yan'
'Yang, Shiping'
'Cui, Yong'
_publ_section_title
;
 Chiral porous metal-organic frameworks containing μ-oxo-bis[Ti(salan)]
 units for asymmetric cyanation of aldehydes.
;
_journal_issue                   29
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12999
_journal_page_last               13002
_journal_paper_doi               10.1039/c5dt01682g
_journal_volume                  44
_journal_year                    2015
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C41 H52 Br Cd N4 O5.5 Ti'
_chemical_formula_sum            'C41 H52 Br Cd N4 O5.5 Ti'
_chemical_formula_weight         929.07
_space_group_crystal_system      tetragonal
_space_group_IT_number           92
_space_group_name_Hall           'P 4abw 2nw'
_space_group_name_H-M_alt        'P 41 21 2'
_symmetry_space_group_name_Hall  'P 4abw 2nw'
_symmetry_space_group_name_H-M   'P 41 21 2'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/cc14hywg
_audit_creation_date             2015-06-07
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-06-08 deposited with the CCDC.
2015-06-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   26.8901(2)
_cell_length_b                   26.8901(2)
_cell_length_c                   13.2591(3)
_cell_measurement_temperature    173(2)
_cell_volume                     9587.4(2)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.817
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0486
_diffrn_reflns_av_unetI/netI     0.0592
_diffrn_reflns_Laue_measured_fraction_full 0.817
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            24662
_diffrn_reflns_point_group_measured_fraction_full 0.799
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         59.728
_diffrn_reflns_theta_min         3.287
_exptl_absorpt_coefficient_mu    6.282
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.287
_exptl_crystal_description       block
_exptl_crystal_F_000             3800
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.521
_refine_diff_density_min         -1.063
_refine_diff_density_rms         0.109
_refine_ls_abs_structure_details
;
 Flack x determined using 2254 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.045(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     574
_refine_ls_number_reflns         6936
_refine_ls_number_restraints     157
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0775
_refine_ls_R_factor_gt           0.0672
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1500P)²+8.4316P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1965
_refine_ls_wR_factor_ref         0.2117
_reflns_Friedel_coverage         0.742
_reflns_Friedel_fraction_full    0.777
_reflns_Friedel_fraction_max     0.963
_reflns_number_gt                5995
_reflns_number_total             6936
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5dt01682g2.cif
_cod_data_source_block           mof2_sq
_cod_depositor_comments
'Adding full bibliography for 7035520--7035521.cif.'
_cod_original_cell_volume        9587.4(3)
_cod_original_formula_sum        'C41 H52 Br Cd N4 O5.50 Ti'
_cod_database_code               7035521
#BEGIN Tags that were not found in dictionaries:
_shelxl_version_number           2014/6
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.744
_shelx_estimated_absorpt_t_min   0.668
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C34-C28
 1.4 with sigma of 0.02
 O6A-C40A
 1.25 with sigma of 0.02
 O6-C40 = O5-C40
 1.22 with sigma of 0.02
 C40A-C41A
 1.51 with sigma of 0.02
 C41-C40 = C41A-C40A
 1.51 with sigma of 0.02
 O6A-C41A \\sim C41A-O5A
 with sigma of 0.02
3. Restrained planarity
 C22, N3, C19, C20, C18, C21
 with sigma of 0.1
4. Rigid bond restraints
 Cd1, C37
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C28, C34A
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.01
 C34, C35
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.01
 C34, C38
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.01
 N4, C37
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.01
 C37A, N4A
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.01
 C34A, C38A
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.01
 C40, O6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C22A, C21A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C12, C18A
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C18A, C19A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C35A, C34A
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.01
 O5, N4
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.01
 O5, C40
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 O5, C40
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C40, C41
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C37A, N4A
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.01
 C38A, C34A
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.01
 C20A
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.01
 N3A, C21A
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
Cd1A \\sim O6: within 1.7A with sigma of 0.001 and sigma for terminal atoms of
0.08
C37 \\sim C38: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
Cd1 \\sim C37: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C35 \\sim C36: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C34 \\sim C35: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C34 \\sim C38: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C28 \\sim C34A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C28 \\sim C34: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C34A \\sim C38A: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.08
C40 \\sim O6: within 1.7A with sigma of 0.001 and sigma for terminal atoms of
1.7
C40 \\sim O6: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.08
O6A \\sim C40A: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.08
C22A \\sim C21A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C12 \\sim C18A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C18A \\sim C19A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C35A \\sim C34A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C36A \\sim C35A: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.08
O5 \\sim N4: within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.08
O5 \\sim C40: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.08
O5A \\sim C40A: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.08
C40 \\sim C41: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.08
C41A \\sim C40A: within 1.7A with sigma of 0.005 and sigma for terminal atoms
of 0.08
Uanis(O5) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.2
Uanis(C37A) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.2
Uanis(C40A) = Uanis(C40)
Uanis(O6) = Uanis(O6A)
Uanis(C41A) = Uanis(C41)
Uanis(C41A) = Uanis(C41)
6. Rigid body (RIGU) restrains
 C18A, C12
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C22A, C21A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Others
 Sof(Cd1A)=Sof(Br1A)=Sof(O6A)=Sof(O5A)=Sof(C41A)=Sof(H41D)=Sof(H41E)=Sof(H41F)=
 Sof(C40A)=Sof(N4A)=Sof(C36A)=Sof(H36A)=Sof(C35A)=Sof(H35A)=Sof(C34A)=Sof(C38A)=
 Sof(H38A)=Sof(C37A)=Sof(H37A)=Sof(C22A)=Sof(H22A)=Sof(C18A)=Sof(C19A)=
 Sof(H19A)=Sof(C20A)=Sof(H20A)=Sof(N3A)=Sof(C21A)=Sof(H21A)=1-FVAR(1)
 Sof(Cd1)=Sof(C22)=Sof(H22)=Sof(Br1)=Sof(O5)=Sof(C40)=Sof(O6)=Sof(C41)=
 Sof(H41A)=Sof(H41B)=Sof(H41C)=Sof(C38)=Sof(H38)=Sof(C34)=Sof(C35)=Sof(H35)=
 Sof(C36)=Sof(H36)=Sof(N4)=Sof(C37)=Sof(H37)=Sof(N3)=Sof(C19)=Sof(H19)=Sof(C20)=
 Sof(H20)=Sof(C18)=Sof(C21)=Sof(H21)=FVAR(1)
8.a Ternary CH refined with riding coordinates:
 N0AA(H0AA), N2(H2), C3AA(H3AA), C2AA(H2AA)
8.b Secondary CH2 refined with riding coordinates:
 C23(H23A,H23B), C1AA(H1AA,H1AB), C7AA(H7AA,H7AB), C5(H5A,H5B), C8AA(H8AA,
 H8AB), C5AA(H5AA,H5AB)
8.c Me refined with riding coordinates:
 C39(H39A,H39B,H39C), C41(H41A,H41B,H41C), C41A(H41D,H41E,H41F)
8.d Aromatic/amide H refined with riding coordinates:
 C11(H11), C13(H13), C29(H29), C4AA(H4AA), C22(H22), C38(H38), C35(H35),
 C36(H36), C37(H37), C36A(H36A), C35A(H35A), C38A(H38A), C37A(H37A), C19(H19),
 C20(H20), C21(H21), C22A(H22A), C19A(H19A), C20A(H20A), C21A(H21A)
8.e Fitted hexagon refined as free rotating group:
 C11(C6AA,C9,C8,C13,C12), C29(C28,C4AA,C26,C24,C25), C38(C34,C35,C36,N4,C37),
 N4A(C36A,C35A,C34A,C38A,C37A), C22A(C18A,C19A,C20A,N3A,C21A)
8.f Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C32(H32A,H32B,H32C), C31(H31A,H31B,H31C), C33(H33A,H33B,
 H33C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C)
;
_olex2_submission_special_instructions 'No special instructions were received'
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y+1/2, x+1/2, z+1/4'
'-x, -y, z+1/2'
'y+1/2, -x+1/2, z+3/4'
'x+1/2, -y+1/2, -z+3/4'
'-x+1/2, y+1/2, -z+1/4'
'y, x, -z'
'-y, -x, -z+1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti1 Ti 0.30573(5) 0.77418(6) 0.67871(13) 0.0359(4) Uani 1 1 d . . . . .
O4 O 0.2871(2) 0.8209(2) 0.7752(5) 0.0427(14) Uani 1 1 d . . . . .
O0AA O 0.3225(2) 0.8257(2) 0.5809(5) 0.0395(14) Uani 1 1 d . . . . .
N0AA N 0.2367(3) 0.7732(3) 0.5898(6) 0.0429(18) Uani 1 1 d . . . . .
H0AA H 0.2117 0.7538 0.6297 0.051 Uiso 1 1 calc R . . . .
N2 N 0.3208(3) 0.7162(3) 0.5589(6) 0.0423(18) Uani 1 1 d . . . . .
H2 H 0.3437 0.7310 0.5077 0.051 Uiso 1 1 calc R . . . .
O3 O 0.2763(2) 0.7237(2) 0.7500 0.0379(19) Uani 1 2 d S T P . .
O1AA O 0.3722(2) 0.7625(2) 0.7095(5) 0.0418(15) Uani 1 1 d . . . . .
C3AA C 0.2743(4) 0.7008(4) 0.5066(7) 0.047(2) Uani 1 1 d . . . . .
H3AA H 0.2559 0.6775 0.5521 0.056 Uiso 1 1 calc R . . . .
C23 C 0.3458(4) 0.6715(4) 0.6036(8) 0.048(2) Uani 1 1 d . . . . .
H23A H 0.3519 0.6472 0.5490 0.058 Uiso 1 1 calc R . . . .
H23B H 0.3226 0.6559 0.6521 0.058 Uiso 1 1 calc R . . . .
C11 C 0.30286(19) 0.9107(2) 0.3729(4) 0.046(2) Uani 1 1 d . . . . .
H11 H 0.3215 0.9299 0.3260 0.055 Uiso 1 1 calc R . . . .
C6AA C 0.32723(14) 0.8820(2) 0.4447(5) 0.041(2) Uani 1 1 d G . . . .
C9 C 0.29993(17) 0.85402(19) 0.5132(4) 0.037(2) Uani 1 1 d G . . . .
C8 C 0.24827(17) 0.8547(2) 0.5099(4) 0.046(2) Uani 1 1 d G . . . .
C13 C 0.22390(14) 0.8834(2) 0.4381(5) 0.053(3) Uani 1 1 d G . . . .
H13 H 0.1886 0.8839 0.4359 0.064 Uiso 1 1 calc R . . . .
C12 C 0.25120(19) 0.9114(2) 0.3696(5) 0.051(3) Uani 1 1 d G U . . .
C29 C 0.4276(2) 0.64177(19) 0.6613(5) 0.056(3) Uani 1 1 d . . . . .
H29 H 0.4202 0.6118 0.6265 0.067 Uiso 1 1 calc R . . . .
C28 C 0.4715(2) 0.6460(2) 0.7160(6) 0.063(3) Uani 1 1 d DG U . . .
C4AA C 0.48229(18) 0.6899(2) 0.7669(5) 0.060(3) Uani 1 1 d G . . . .
H4AA H 0.5123 0.6927 0.8043 0.072 Uiso 1 1 calc R . . . .
C26 C 0.4492(2) 0.7295(2) 0.7630(5) 0.048(2) Uani 1 1 d G . . . .
C24 C 0.40535(18) 0.72534(18) 0.7083(5) 0.043(2) Uani 1 1 d G . . . .
C25 C 0.39454(18) 0.6815(2) 0.6574(5) 0.047(2) Uani 1 1 d G . . . .
C39 C 0.2972(5) 0.8720(4) 0.7846(10) 0.068(3) Uani 1 1 d . . . . .
H39A H 0.2811 0.8849 0.8457 0.102 Uiso 1 1 calc R . . . .
H39B H 0.3332 0.8772 0.7893 0.102 Uiso 1 1 calc R . . . .
H39C H 0.2842 0.8897 0.7255 0.102 Uiso 1 1 calc R . . . .
Cd1 Cd 0.62627(10) 0.45282(11) 0.7111(3) 0.0652(10) Uani 0.545(7) 1 d . U . A 1
C1AA C 0.2172(3) 0.8247(3) 0.5815(9) 0.049(2) Uani 1 1 d . . . . .
H1AA H 0.2175 0.8406 0.6488 0.058 Uiso 1 1 calc R . . . .
H1AB H 0.1824 0.8238 0.5572 0.058 Uiso 1 1 calc R . . . .
C14 C 0.3856(3) 0.8822(4) 0.4487(8) 0.045(2) Uani 1 1 d . . . . .
C7AA C 0.2816(5) 0.6753(4) 0.4069(8) 0.064(3) Uani 1 1 d . . . . .
H7AA H 0.3010 0.6444 0.4172 0.077 Uiso 1 1 calc R . . . .
H7AB H 0.3008 0.6973 0.3615 0.077 Uiso 1 1 calc R . . . .
C30 C 0.4617(3) 0.7791(5) 0.8204(9) 0.057(3) Uani 1 1 d . . . . .
C15 C 0.4052(4) 0.8283(4) 0.4354(10) 0.062(3) Uani 1 1 d . . . . .
H15A H 0.3956 0.8083 0.4941 0.093 Uiso 1 1 calc GR . . . .
H15B H 0.4415 0.8288 0.4295 0.093 Uiso 1 1 calc GR . . . .
H15C H 0.3908 0.8137 0.3743 0.093 Uiso 1 1 calc GR . . . .
C5 C 0.1986(6) 0.7075(5) 0.3460(10) 0.080(4) Uani 1 1 d . . . . .
H5A H 0.2133 0.7303 0.2955 0.096 Uiso 1 1 calc R . . . .
H5B H 0.1658 0.6965 0.3201 0.096 Uiso 1 1 calc R . . . .
C2AA C 0.2422(4) 0.7475(4) 0.4917(8) 0.049(2) Uani 1 1 d . . . . .
H2AA H 0.2604 0.7704 0.4452 0.059 Uiso 1 1 calc R . . . .
C32 C 0.4613(4) 0.8229(4) 0.7504(10) 0.057(3) Uani 1 1 d . . . . .
H32A H 0.4879 0.8192 0.7003 0.085 Uiso 1 1 calc GR . . . .
H32B H 0.4667 0.8535 0.7891 0.085 Uiso 1 1 calc GR . . . .
H32C H 0.4291 0.8247 0.7159 0.085 Uiso 1 1 calc GR . . . .
C31 C 0.5142(4) 0.7766(6) 0.8747(10) 0.071(3) Uani 1 1 d . . . . .
H31A H 0.5157 0.7469 0.9174 0.106 Uiso 1 1 calc GR . . . .
H31B H 0.5188 0.8064 0.9164 0.106 Uiso 1 1 calc GR . . . .
H31C H 0.5406 0.7751 0.8237 0.106 Uiso 1 1 calc GR . . . .
C33 C 0.4227(4) 0.7870(5) 0.9039(9) 0.065(3) Uani 1 1 d . . . . .
H33A H 0.3904 0.7944 0.8732 0.097 Uiso 1 1 calc GR . . . .
H33B H 0.4329 0.8148 0.9469 0.097 Uiso 1 1 calc GR . . . .
H33C H 0.4200 0.7567 0.9448 0.097 Uiso 1 1 calc GR . . . .
C8AA C 0.1913(4) 0.7347(4) 0.4419(9) 0.065(3) Uani 1 1 d . . . . .
H8AA H 0.1714 0.7141 0.4888 0.078 Uiso 1 1 calc R . . . .
H8AB H 0.1727 0.7658 0.4288 0.078 Uiso 1 1 calc R . . . .
C16 C 0.4025(4) 0.9037(4) 0.5459(9) 0.057(3) Uani 1 1 d . . . . .
H16A H 0.3894 0.9375 0.5529 0.085 Uiso 1 1 calc GR . . . .
H16B H 0.4389 0.9046 0.5473 0.085 Uiso 1 1 calc GR . . . .
H16C H 0.3904 0.8831 0.6017 0.085 Uiso 1 1 calc GR . . . .
C22 C 0.2330(13) 0.9903(16) 0.280(2) 0.054(10) Uani 0.545(7) 1 d . . . A 1
H22 H 0.2620 1.0044 0.3097 0.065 Uiso 0.545(7) 1 calc R . . A 1
C17 C 0.4081(5) 0.9125(5) 0.3629(11) 0.079(4) Uani 1 1 d . . . . .
H17A H 0.4053 0.8938 0.2997 0.118 Uiso 1 1 calc GR . . . .
H17B H 0.4433 0.9190 0.3774 0.118 Uiso 1 1 calc GR . . . .
H17C H 0.3903 0.9441 0.3565 0.118 Uiso 1 1 calc GR . . . .
C5AA C 0.2321(6) 0.6624(5) 0.3576(11) 0.079(4) Uani 1 1 d . . . . .
H5AA H 0.2385 0.6477 0.2904 0.094 Uiso 1 1 calc R . . . .
H5AB H 0.2149 0.6370 0.3991 0.094 Uiso 1 1 calc R . . . .
Br1 Br 0.5917(2) 0.3975(3) 0.8692(6) 0.138(2) Uani 0.545(7) 1 d . . . . .
O5 O 0.7058(9) 0.4265(8) 0.7418(17) 0.096(5) Uani 0.545(7) 1 d D U . A 1
Cd1A Cd 0.64210(13) 0.47139(15) 0.7648(4) 0.0725(13) Uani 0.455(7) 1 d . U . A
2
C40 C 0.7155(9) 0.4666(9) 0.790(2) 0.0764(17) Uani 0.545(7) 1 d D U . A 1
Br1A Br 0.6036(2) 0.4258(3) 0.9259(6) 0.112(2) Uani 0.455(7) 1 d . . . A .
O6 O 0.6848(6) 0.4982(6) 0.8129(14) 0.0757(15) Uani 0.545(7) 1 d D U . A 1
C41 C 0.7683(12) 0.4769(18) 0.822(4) 0.119(11) Uani 0.545(7) 1 d D U . A 1
H41A H 0.7897 0.4495 0.7998 0.179 Uiso 0.545(7) 1 calc R . . A 1
H41B H 0.7797 0.5080 0.7905 0.179 Uiso 0.545(7) 1 calc R . . A 1
H41C H 0.7699 0.4801 0.8952 0.179 Uiso 0.545(7) 1 calc R . . A 1
O6A O 0.6998(7) 0.5240(7) 0.8629(16) 0.0757(15) Uani 0.455(7) 1 d D U . A 2
O5A O 0.7184(8) 0.4463(9) 0.786(2) 0.089(5) Uani 0.455(7) 1 d D U . A 2
C41A C 0.7831(12) 0.4974(17) 0.845(4) 0.119(11) Uani 0.455(7) 1 d D U . A 2
H41D H 0.8009 0.4676 0.8221 0.179 Uiso 0.455(7) 1 calc R . . A 2
H41E H 0.7927 0.5258 0.8033 0.179 Uiso 0.455(7) 1 calc R . . A 2
H41F H 0.7916 0.5041 0.9156 0.179 Uiso 0.455(7) 1 calc R . . A 2
C40A C 0.7278(10) 0.4889(10) 0.836(3) 0.0764(17) Uani 0.455(7) 1 d D U . A 2
C38 C 0.4998(7) 0.5620(7) 0.6365(15) 0.057(7) Uani 0.545(7) 1 d . U . A 1
H38 H 0.4767 0.5650 0.5827 0.068 Uiso 0.545(7) 1 calc R . . A 1
C34 C 0.5024(10) 0.5987(8) 0.710(2) 0.059(7) Uani 0.545(7) 1 d DG U . A 1
C35 C 0.5362(11) 0.5943(9) 0.789(2) 0.082(9) Uani 0.545(7) 1 d G U . A 1
H35 H 0.5379 0.6194 0.8392 0.098 Uiso 0.545(7) 1 calc R . . A 1
C36 C 0.5674(9) 0.5532(8) 0.7941(17) 0.083(10) Uani 0.545(7) 1 d G U . A 1
H36 H 0.5905 0.5502 0.8480 0.100 Uiso 0.545(7) 1 calc R . . A 1
N4 N 0.5648(7) 0.5165(6) 0.7205(15) 0.067(7) Uani 0.545(7) 1 d G U . A 1
C37 C 0.5310(6) 0.5209(6) 0.6417(12) 0.058(5) Uani 0.545(7) 1 d G U . A 1
H37 H 0.5292 0.4958 0.5914 0.069 Uiso 0.545(7) 1 calc R . . A 1
N4A N 0.5797(8) 0.5277(8) 0.7566(17) 0.052(6) Uani 0.455(7) 1 d . U . A 2
C36A C 0.5766(10) 0.5633(9) 0.8323(16) 0.075(9) Uani 0.455(7) 1 d G U . A 2
H36A H 0.5977 0.5612 0.8896 0.090 Uiso 0.455(7) 1 calc R . . A 2
C35A C 0.5425(12) 0.6019(10) 0.8243(19) 0.068(8) Uani 0.455(7) 1 d G U . A 2
H35A H 0.5403 0.6263 0.8760 0.082 Uiso 0.455(7) 1 calc R . . A 2
C34A C 0.5116(10) 0.6050(9) 0.741(2) 0.051(7) Uani 0.455(7) 1 d G U . A 2
C38A C 0.5147(9) 0.5694(9) 0.6648(17) 0.052(7) Uani 0.455(7) 1 d G U . A 2
H38A H 0.4936 0.5715 0.6075 0.063 Uiso 0.455(7) 1 calc R . . A 2
C37A C 0.5488(9) 0.5307(8) 0.6728(16) 0.065(9) Uani 0.455(7) 1 d G U . A 2
H37A H 0.5509 0.5064 0.6211 0.078 Uiso 0.455(7) 1 calc R . . A 2
N3 N 0.1666(9) 1.0024(8) 0.1764(16) 0.059(6) Uani 0.545(7) 1 d . . . A 1
C19 C 0.1779(8) 0.9282(9) 0.2586(19) 0.056(7) Uani 0.545(7) 1 d . . . A 1
H19 H 0.1661 0.8956 0.2727 0.067 Uiso 0.545(7) 1 calc R . . A 1
C20 C 0.1521(10) 0.9571(10) 0.195(2) 0.077(9) Uani 0.545(7) 1 d . . . A 1
H20 H 0.1230 0.9444 0.1638 0.092 Uiso 0.545(7) 1 calc R . . A 1
C18 C 0.2196(10) 0.9436(10) 0.3026(18) 0.040(7) Uani 0.545(7) 1 d . . . A 1
C21 C 0.2054(13) 1.0169(11) 0.216(2) 0.057(9) Uani 0.545(7) 1 d . . . A 1
H21 H 0.2165 1.0495 0.2005 0.069 Uiso 0.545(7) 1 calc R . . A 1
C22A C 0.2396(11) 0.9880(11) 0.256(2) 0.032(8) Uani 0.455(7) 1 d . U . A 2
H22A H 0.2646 1.0050 0.2928 0.039 Uiso 0.455(7) 1 calc R . . A 2
C18A C 0.2298(9) 0.9382(10) 0.2757(18) 0.049(9) Uani 0.455(7) 1 d G U . A 2
C19A C 0.1932(9) 0.9133(6) 0.2217(19) 0.056(7) Uani 0.455(7) 1 d G U . A 2
H19A H 0.1865 0.8793 0.2352 0.067 Uiso 0.455(7) 1 calc R . . A 2
C20A C 0.1662(9) 0.9383(7) 0.1479(18) 0.074(10) Uani 0.455(7) 1 d G U . A 2
H20A H 0.1412 0.9213 0.1110 0.089 Uiso 0.455(7) 1 calc R . . A 2
N3A N 0.1760(10) 0.9881(7) 0.1281(17) 0.064(9) Uani 0.455(7) 1 d G U . A 2
C21A C 0.2126(12) 1.0130(7) 0.182(2) 0.049(10) Uani 0.455(7) 1 d G U . A 2
H21A H 0.2193 1.0470 0.1685 0.058 Uiso 0.455(7) 1 calc R . . A 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd 0.1185 4.6533 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2191 1.8069 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O4 Ti1 O0AA 92.3(3) . .
O4 Ti1 N0AA 98.6(3) . .
O4 Ti1 N2 174.7(3) . .
O0AA Ti1 N0AA 81.2(3) . .
O0AA Ti1 N2 88.9(3) . .
N0AA Ti1 N2 76.5(3) . .
O3 Ti1 O4 91.7(3) . .
O3 Ti1 O0AA 165.5(2) . .
O3 Ti1 N0AA 84.4(2) . .
O3 Ti1 N2 85.9(2) . .
O3 Ti1 O1AA 100.1(3) . .
O1AA Ti1 O4 102.8(3) . .
O1AA Ti1 O0AA 92.6(3) . .
O1AA Ti1 N0AA 157.9(3) . .
O1AA Ti1 N2 82.3(3) . .
C39 O4 Ti1 132.0(7) . .
C9 O0AA Ti1 139.0(4) . .
C1AA N0AA Ti1 109.0(6) . .
C2AA N0AA Ti1 113.1(6) . .
C2AA N0AA C1AA 113.9(8) . .
C3AA N2 Ti1 111.6(6) . .
C3AA N2 C23 109.7(7) . .
C23 N2 Ti1 110.8(6) . .
Ti1 O3 Ti1 154.7(5) . 8_666
C24 O1AA Ti1 139.7(5) . .
N2 C3AA C7AA 115.3(9) . .
N2 C3AA C2AA 107.7(7) . .
C7AA C3AA C2AA 109.4(8) . .
N2 C23 C25 115.7(8) . .
C6AA C11 C12 120.0 . .
C11 C6AA C9 120.0 . .
C11 C6AA C14 119.5(5) . .
C9 C6AA C14 120.5(5) . .
O0AA C9 C6AA 120.9(4) . .
O0AA C9 C8 119.1(4) . .
C8 C9 C6AA 120.0 . .
C9 C8 C13 120.0 . .
C9 C8 C1AA 122.0(5) . .
C13 C8 C1AA 118.0(5) . .
C8 C13 C12 120.0 . .
C11 C12 C18 126.2(11) . .
C11 C12 C18A 113.7(11) . .
C13 C12 C11 120.0 . .
C13 C12 C18 113.6(11) . .
C13 C12 C18A 125.6(11) . .
C28 C29 C25 120.0 . .
C29 C28 C4AA 120.0 . .
C29 C28 C34 111.7(9) . .
C29 C28 C34A 129.2(11) . .
C4AA C28 C34 128.3(9) . .
C4AA C28 C34A 110.5(10) . .
C26 C4AA C28 120.0 . .
C4AA C26 C30 119.8(5) . .
C24 C26 C4AA 120.0 . .
C24 C26 C30 120.2(5) . .
O1AA C24 C26 119.9(5) . .
O1AA C24 C25 120.0(5) . .
C26 C24 C25 120.0 . .
C29 C25 C23 115.8(5) . .
C24 C25 C23 123.9(5) . .
C24 C25 C29 120.0 . .
Br1 Cd1 Cd1 32.8(2) . 8_666
Br1 Cd1 Cd1 59.2(2) 8_666 8_666
Br1 Cd1 Br1 88.3(3) 8_666 .
Br1 Cd1 O5 104.0(6) 8_666 .
Br1 Cd1 C40 132.7(6) 8_666 .
Br1 Cd1 Br1A 11.7(3) 8_666 8_666
Br1 Cd1 Br1A 21.78(15) . .
Br1 Cd1 Br1A 110.0(3) 8_666 .
Br1 Cd1 Br1A 91.9(2) . 8_666
Br1 Cd1 O6 160.2(4) 8_666 .
Br1 Cd1 N4 105.9(5) 8_666 .
Br1 Cd1 N3 92.7(6) 8_666 5_565
O5 Cd1 Cd1 111.1(6) . 8_666
O5 Cd1 Br1 90.8(6) . .
O5 Cd1 C40 29.0(5) . .
O5 Cd1 Br1A 86.9(6) . .
O5 Cd1 Br1A 115.0(6) . 8_666
O5 Cd1 O6 56.3(6) . .
O5 Cd1 N4 149.4(7) . .
O5 Cd1 N3 82.5(8) . 5_565
C40 Cd1 Cd1 124.9(7) . 8_666
C40 Cd1 Br1 94.7(7) . .
C40 Cd1 Br1A 143.2(5) . 8_666
C40 Cd1 Br1A 81.0(7) . .
Br1A Cd1 Cd1 60.33(18) 8_666 8_666
Br1A Cd1 Cd1 52.7(2) . 8_666
Br1A Cd1 Br1A 112.92(18) 8_666 .
O6 Cd1 Cd1 126.5(4) . 8_666
O6 Cd1 Br1 93.9(4) . .
O6 Cd1 C40 27.5(5) . .
O6 Cd1 Br1A 74.0(4) . .
O6 Cd1 Br1A 169.6(4) . 8_666
O6 Cd1 N3 83.0(6) . 5_565
N4 Cd1 Cd1 90.0(5) . 8_666
N4 Cd1 Br1 96.6(5) . .
N4 Cd1 C40 120.5(7) . .
N4 Cd1 Br1A 89.0(5) . .
N4 Cd1 Br1A 94.5(5) . 8_666
N4 Cd1 O6 93.4(6) . .
N4 Cd1 N3 89.6(8) . 5_565
N3 Cd1 Cd1 150.5(6) 5_565 8_666
N3 Cd1 Br1 173.3(6) 5_565 .
N3 Cd1 C40 79.8(9) 5_565 .
N3 Cd1 Br1A 156.8(6) 5_565 .
N3 Cd1 Br1A 90.3(5) 5_565 8_666
N0AA C1AA C8 110.7(7) . .
C15 C14 C6AA 109.5(8) . .
C16 C14 C6AA 109.7(8) . .
C16 C14 C15 111.0(9) . .
C16 C14 C17 108.5(9) . .
C17 C14 C6AA 111.9(8) . .
C17 C14 C15 106.2(9) . .
C3AA C7AA C5AA 111.6(11) . .
C26 C30 C31 112.0(9) . .
C32 C30 C26 111.4(9) . .
C32 C30 C31 108.7(9) . .
C32 C30 C33 109.4(10) . .
C33 C30 C26 108.7(8) . .
C33 C30 C31 106.6(10) . .
C8AA C5 C5AA 112.7(11) . .
N0AA C2AA C3AA 108.9(8) . .
N0AA C2AA C8AA 112.8(9) . .
C3AA C2AA C8AA 111.6(8) . .
C5 C8AA C2AA 110.9(11) . .
C21 C22 C18 119(3) . .
C5 C5AA C7AA 112.4(11) . .
Cd1 Br1 Cd1 87.9(2) 8_666 .
Cd1A Br1 Cd1A 105.2(2) 8_666 .
Br1A Br1 Cd1 92.7(5) . .
Br1A Br1 Cd1 150.1(6) . 8_666
Br1A Br1 Cd1A 73.0(4) . .
Br1A Br1 Cd1A 154.1(6) . 8_666
C40 O5 Cd1 91.1(16) . .
Br1 Cd1A Br1 71.5(2) 8_666 .
Br1A Cd1A Br1 94.9(2) . 8_666
Br1A Cd1A Br1 23.53(16) . .
O6A Cd1A Br1 117.0(4) . .
O6A Cd1A Br1 164.2(4) . 8_666
O6A Cd1A Br1A 94.9(5) . .
O6A Cd1A C40A 29.1(6) . .
O5A Cd1A Br1 100.0(5) . .
O5A Cd1A Br1 105.3(9) . 8_666
O5A Cd1A Br1A 96.8(6) . .
O5A Cd1A O6A 61.1(9) . .
O5A Cd1A C40A 32.1(9) . .
O5A Cd1A N4A 155.8(10) . .
O5A Cd1A N3A 83(7) . 5_565
C40A Cd1A Br1 113.0(6) . .
C40A Cd1A Br1 136.6(6) . 8_666
C40A Cd1A Br1A 98.0(7) . .
N4A Cd1A Br1 95.6(6) . 8_666
N4A Cd1A Br1 98.1(6) . .
N4A Cd1A Br1A 93.3(6) . .
N4A Cd1A O6A 96.2(7) . .
N4A Cd1A C40A 124.6(8) . .
N4A Cd1A N3A 86(7) . 5_565
N3A Cd1A Br1 156(6) 5_565 .
N3A Cd1A Br1 85(6) 5_565 8_666
N3A Cd1A Br1A 180(7) 5_565 .
N3A Cd1A O6A 85(6) 5_565 .
N3A Cd1A C40A 82(6) 5_565 .
O5 C40 Cd1 60.0(15) . .
O5 C40 C41 119(3) . .
O6 C40 Cd1 65.4(14) . .
O6 C40 O5 125(2) . .
O6 C40 C41 116(3) . .
C41 C40 Cd1 173(3) . .
Cd1 Br1A Cd1 66.97(18) 8_666 .
Br1 Br1A Cd1 65.5(4) . .
Br1 Br1A Cd1 18.2(4) . 8_666
Br1 Br1A Cd1A 83.5(5) . .
C40 O6 Cd1 87.1(16) . .
C40A O6A Cd1A 78.3(19) . .
C40A O5A Cd1A 88.8(15) . .
O6A C40A Cd1A 72.6(18) . .
O6A C40A O5A 132(3) . .
O6A C40A C41A 117(3) . .
O5A C40A Cd1A 59.2(15) . .
O5A C40A C41A 110.7(19) . .
C41A C40A Cd1A 162(3) . .
C34 C38 C37 120.0 . .
C38 C34 C28 127.0(12) . .
C35 C34 C28 113.0(12) . .
C35 C34 C38 120.0 . .
C34 C35 C36 120.0 . .
N4 C36 C35 120.0 . .
C36 N4 Cd1 120.8(9) . .
C36 N4 C37 120.0 . .
C37 N4 Cd1 118.4(9) . .
N4 C37 C38 120.0 . .
C36A N4A Cd1A 118.1(11) . .
C36A N4A C37A 120.0 . .
C37A N4A Cd1A 121.5(11) . .
N4A C36A C35A 120.0 . .
C34A C35A C36A 120.0 . .
C35A C34A C28 128.0(14) . .
C38A C34A C28 112.0(14) . .
C38A C34A C35A 120.0 . .
C37A C38A C34A 120.0 . .
C38A C37A N4A 120.0 . .
C20 N3 Cd1 118.2(19) . 5_465
C21 N3 Cd1 123(2) . 5_465
C21 N3 C20 118(2) . .
C18 C19 C20 122(2) . .
N3 C20 C19 121(2) . .
C22 C18 C12 121(2) . .
C19 C18 C12 124(2) . .
C19 C18 C22 115(2) . .
N3 C21 C22 125(3) . .
C18A C22A C21A 120.0 . .
C22A C18A C12 122.0(17) . .
C22A C18A C19A 120.0 . .
C19A C18A C12 117.0(17) . .
C20A C19A C18A 120.0 . .
C19A C20A N3A 120.0 . .
C20A N3A Cd1A 121.5(11) . 5_465
C20A N3A C21A 120.0 . .
C21A N3A Cd1A 117.6(11) . 5_465
N3A C21A C22A 120.0 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ti1 O4 1.861(7) .
Ti1 O0AA 1.949(6) .
Ti1 N0AA 2.200(8) .
Ti1 N2 2.263(8) .
Ti1 O3 1.834(2) .
Ti1 O1AA 1.860(6) .
O4 C39 1.407(13) .
O0AA C9 1.324(7) .
N0AA C1AA 1.485(12) .
N0AA C2AA 1.479(14) .
N2 C3AA 1.489(12) .
N2 C23 1.497(12) .
O3 Ti1 1.834(2) 8_666
O1AA C24 1.339(7) .
C3AA C7AA 1.502(16) .
C3AA C2AA 1.538(14) .
C23 C25 1.516(11) .
C11 C6AA 1.3900 .
C11 C12 1.3900 .
C6AA C9 1.3900 .
C6AA C14 1.570(10) .
C9 C8 1.3900 .
C8 C13 1.3900 .
C8 C1AA 1.499(11) .
C13 C12 1.3900 .
C12 C18 1.50(2) .
C12 C18A 1.548(18) .
C29 C28 1.3900 .
C29 C25 1.3900 .
C28 C4AA 1.3900 .
C28 C34 1.520(13) .
C28 C34A 1.575(19) .
C4AA C26 1.3900 .
C26 C24 1.3900 .
C26 C30 1.571(14) .
C24 C25 1.3900 .
Cd1 Cd1 3.180(5) 8_666
Cd1 Br1 2.735(5) .
Cd1 Br1 1.725(13) 8_666
Cd1 O5 2.29(2) .
Cd1 C40 2.64(3) .
Cd1 Br1A 3.002(6) .
Cd1 Br1A 2.748(13) 8_666
Cd1 O6 2.41(2) .
Cd1 N4 2.383(14) .
Cd1 N3 2.44(2) 5_565
C14 C15 1.552(14) .
C14 C16 1.484(16) .
C14 C17 1.525(15) .
C7AA C5AA 1.52(2) .
C30 C32 1.501(16) .
C30 C31 1.586(14) .
C30 C33 1.539(16) .
C5 C8AA 1.48(2) .
C5 C5AA 1.52(2) .
C2AA C8AA 1.557(14) .
C22 C18 1.34(4) .
C22 C21 1.33(3) .
Br1 Cd1 1.725(13) 8_666
Br1 Cd1A 2.677(14) 8_666
Br1 Cd1A 2.776(6) .
Br1 Br1A 1.116(8) .
O5 C40 1.28(2) .
Cd1A Br1 2.677(14) 8_666
Cd1A Br1A 2.672(5) .
Cd1A O6A 2.47(3) .
Cd1A O5A 2.177(19) .
Cd1A C40A 2.54(3) .
Cd1A N4A 2.262(18) .
Cd1A N3A 2.37(18) 5_565
C40 O6 1.22(2) .
C40 C41 1.51(2) .
Br1A Cd1 2.748(13) 8_666
O6A C40A 1.26(2) .
O5A C40A 1.35(4) .
C41A C40A 1.508(19) .
C38 C34 1.3900 .
C38 C37 1.3900 .
C34 C35 1.3900 .
C35 C36 1.3900 .
C36 N4 1.3900 .
N4 C37 1.3900 .
N4A C36A 1.3900 .
N4A C37A 1.3900 .
C36A C35A 1.3900 .
C35A C34A 1.3900 .
C34A C38A 1.3900 .
C38A C37A 1.3900 .
N3 Cd1 2.44(2) 5_465
N3 C20 1.30(3) .
N3 C21 1.23(3) .
C19 C20 1.34(4) .
C19 C18 1.33(3) .
C22A C18A 1.3900 .
C22A C21A 1.3900 .
C18A C19A 1.3900 .
C19A C20A 1.3900 .
C20A N3A 1.3900 .
N3A Cd1A 2.368(16) 5_465
N3A C21A 1.3900 .
