#------------------------------------------------------------------------------
#$Date: 2018-12-20 01:18:44 +0200 (Thu, 20 Dec 2018) $
#$Revision: 212667 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/03/1550380.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_1550380
loop_
_publ_author_name
'Feng, Xuanyu'
'Song, Yang'
'Chen, Justin S.'
'Li, Zhe'
'Chen, Emily Y.'
'Kaufmann, Michael'
'Wang, Cheng'
'Lin, Wenbin'
_publ_section_title
;
 Cobalt-Bridged Secondary Building Units in a Titanium Metal-Organic
 Framework Catalyze Cascade Reduction of N-Heteroarenes
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C8SC04610G
_journal_year                    2019
_chemical_compound_source        No
_chemical_formula_moiety         '0.67(C63 H37.5 O21 Ti4.5)'
_chemical_formula_sum            'C42 H30 O14 Ti3'
_chemical_formula_weight         902.36
_chemical_name_common            Ti3-BPDC
_chemical_name_systematic        Ti3-BPDC
_space_group_crystal_system      trigonal
_space_group_IT_number           166
_space_group_name_Hall           '-R 3 2"'
_space_group_name_H-M_alt        'R -3 m'
_symmetry_space_group_name_Hall  '-R 3 2"'
_symmetry_space_group_name_H-M   'R -3 m :H'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-07-13
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-07-29 deposited with the CCDC.
2018-12-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   25.8366(16)
_cell_length_b                   25.8366(16)
_cell_length_c                   13.6675(9)
_cell_measurement_reflns_used    8282
_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      49.454
_cell_measurement_theta_min      4.706
_cell_volume                     7901.2(9)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.96
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0293
_diffrn_reflns_av_unetI/netI     0.0157
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            16826
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        24.727
_diffrn_reflns_theta_max         24.727
_diffrn_reflns_theta_min         2.353
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.248
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_correction_T_min  0.5804
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.0802 before and 0.0448 after correction.
The Ratio of minimum to maximum transmission is 0.7790.
The λ/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.569
_exptl_crystal_description       Cubic
_exptl_crystal_F_000             1380
_exptl_crystal_preparation       Catalysis
_exptl_crystal_recrystallization_method Solvothermal
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.976
_refine_diff_density_min         -1.412
_refine_diff_density_rms         0.095
_refine_ls_extinction_coef       0.0018(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.607
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     64
_refine_ls_number_reflns         1614
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.604
_refine_ls_R_factor_all          0.1213
_refine_ls_R_factor_gt           0.1129
_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)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3430
_refine_ls_wR_factor_ref         0.3547
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1332
_reflns_number_total             1614
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8sc04610g2.cif
_cod_data_source_block           trial2_a
_cod_original_cell_volume        7901.1(11)
_cod_database_code               1550380
_shelx_shelxl_version_number     2014/7
_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.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 O3-H3A
 1 with sigma of 0.96
3. Uiso/Uaniso restraints and constraints
Uanis(O3) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4.a Riding coordinates:
 C6(H3A)
4.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C3(H3), C7(H7), C6(H6)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+1/3'
'x-y+2/3, -y+1/3, -z+1/3'
'-x+2/3, -x+y+1/3, -z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+2/3'
'x-y+1/3, -y+2/3, -z+2/3'
'-x+1/3, -x+y+2/3, -z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z+1/3'
'-x+y+2/3, y+1/3, z+1/3'
'x+2/3, x-y+1/3, z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+2/3'
'-x+y+1/3, y+2/3, z+2/3'
'x+1/3, x-y+2/3, z+2/3'
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
Ti1 Ti 0.3333 0.6667 0.44892(9) 0.0544(7) Uani 1 6 d S T P
Ti2 Ti 0.3333 0.6667 0.1667 0.0725(9) Uani 1 12 d S T P
O1 O 0.29078(12) 0.5816(2) 0.4254(5) 0.128(2) Uani 1 2 d S T P
O2 O 0.29220(15) 0.5844(3) 0.2670(6) 0.178(4) Uani 1 2 d S T P
C1 C 0.27866(18) 0.5573(4) 0.3427(7) 0.117(2) Uani 1 2 d S T P
C2 C 0.24551(17) 0.4910(3) 0.3420(7) 0.139(3) Uani 1 2 d S T P
C5 C 0.1835(2) 0.3669(4) 0.3349(8) 0.161(4) Uani 1 2 d S T P
C4 C 0.1992(2) 0.3985(4) 0.4209(8) 0.165(5) Uani 1 2 d S T P
H4 H 0.1889 0.3777 0.4799 0.198 Uiso 1 2 calc RS T P
C3 C 0.22864(19) 0.4573(4) 0.4222(8) 0.167(5) Uani 1 2 d S T P
H3 H 0.2382 0.4764 0.4827 0.200 Uiso 1 2 calc RS T P
O3 O 0.3333 0.6667 0.5998(19) 0.219(6) Uani 1 6 d DS TU P
C7 C 0.2300(2) 0.4601(5) 0.2563(10) 0.236(9) Uani 1 2 d S T P
H7 H 0.2405 0.4810 0.1975 0.284 Uiso 1 2 calc RS T P
C6 C 0.2009(2) 0.4018(5) 0.2544(10) 0.248(11) Uani 1 2 d S T P
H6 H 0.1916 0.3831 0.1936 0.297 Uiso 1 2 calc RS T P
H3A H 0.3333 0.6667 0.6667 0.297 Uiso 1 12 d DRS T P
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 '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
O1 Ti1 O1 117.28(11) 3_565 .
O1 Ti1 O1 117.28(11) 3_565 2_665
O1 Ti1 O1 117.28(11) . 2_665
O1 Ti1 O3 99.59(19) 3_565 .
O1 Ti1 O3 99.59(19) . .
O1 Ti1 O3 99.6(2) 2_665 .
O2 Ti2 O2 92.0(3) 3_565 26_455
O2 Ti2 O2 180.0 26_455 2_665
O2 Ti2 O2 88.0(3) 3_565 .
O2 Ti2 O2 92.0(3) 3_565 25_565
O2 Ti2 O2 88.0(3) 25_565 27
O2 Ti2 O2 88.0(3) 26_455 25_565
O2 Ti2 O2 88.0(3) 3_565 2_665
O2 Ti2 O2 88.0(3) 26_455 27
O2 Ti2 O2 92.0(3) 25_565 2_665
O2 Ti2 O2 180.0 25_565 .
O2 Ti2 O2 92.0(3) 27 2_665
O2 Ti2 O2 88.0(3) . 2_665
O2 Ti2 O2 92.0(3) 26_455 .
O2 Ti2 O2 92.0(3) . 27
O2 Ti2 O2 180.0 3_565 27
C1 O1 Ti1 125.2(5) . .
C1 O2 Ti2 157.1(7) . .
O1 C1 C2 116.0(7) . .
O2 C1 O1 124.0(8) . .
O2 C1 C2 120.0(9) . .
C3 C2 C1 124.2(9) . .
C3 C2 C7 114.9(8) . .
C7 C2 C1 121.0(8) . .
C4 C5 C5 122.5(10) . 31
C6 C5 C5 123.8(13) . 31
C6 C5 C4 113.7(9) . .
C5 C4 H4 119.1 . .
C3 C4 C5 121.8(9) . .
C3 C4 H4 119.1 . .
C2 C3 H3 118.1 . .
C4 C3 C2 123.7(10) . .
C4 C3 H3 118.1 . .
Ti1 O3 H3A 180.0 . .
C2 C7 H7 119.1 . .
C6 C7 C2 121.7(10) . .
C6 C7 H7 119.1 . .
C5 C6 H6 117.9 . .
C7 C6 C5 124.2(13) . .
C7 C6 H6 117.9 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ti1 O1 1.931(6) 3_565
Ti1 O1 1.931(6) .
Ti1 O1 1.931(6) 2_665
Ti1 O3 2.06(3) .
Ti2 O2 2.296(5) 26_455
Ti2 O2 2.296(5) 25_565
Ti2 O2 2.296(5) 3_565
Ti2 O2 2.296(5) 27
Ti2 O2 2.296(5) 2_665
Ti2 O2 2.296(5) .
O1 C1 1.254(11) .
O2 C1 1.198(10) .
C1 C2 1.483(12) .
C2 C3 1.332(13) .
C2 C7 1.361(15) .
C5 C5 1.504(19) 31
C5 C4 1.372(15) .
C5 C6 1.349(15) .
C4 H4 0.9300 .
C4 C3 1.316(13) .
C3 H3 0.9300 .
O3 H3A 0.9140 .
C7 H7 0.9300 .
C7 C6 1.303(15) .
C6 H6 0.9300 .
