#------------------------------------------------------------------------------
#$Date: 2016-03-21 11:15:17 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178685 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/96/4079685.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_4079685
loop_
_publ_author_name
'Fernández-Galán, Rafael'
'Antiñolo, Antonio'
'Carrillo-Hermosilla, Fernando'
'López-Solera, Isabel'
'Otero, Antonio'
'Serrano-Laguna, Amparo'
'Villaseñor, Elena'
_publ_section_title
;
 Migratory Insertion Reactions in Asymmetrical Guanidinate-Supported
 Zirconium Complexes
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              8360
_journal_paper_doi               10.1021/om300942p
_journal_volume                  31
_journal_year                    2012
_chemical_formula_sum            'C82.5 H104 Br4 N12 Zr2'
_chemical_formula_weight         1765.86
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                103.345(7)
_cell_angle_beta                 93.393(8)
_cell_angle_gamma                95.516(8)
_cell_formula_units_Z            2
_cell_length_a                   9.5720(10)
_cell_length_b                   17.2005(18)
_cell_length_c                   26.670(3)
_cell_measurement_reflns_used    2852
_cell_measurement_temperature    260(2)
_cell_measurement_theta_max      20.1628
_cell_measurement_theta_min      2.5108
_cell_volume                     4237.6(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      260(2)
_diffrn_measured_fraction_theta_full 0.956
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0746
_diffrn_reflns_av_sigmaI/netI    0.2573
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            41263
_diffrn_reflns_theta_full        30.59
_diffrn_reflns_theta_max         30.59
_diffrn_reflns_theta_min         1.61
_exptl_absorpt_coefficient_mu    2.180
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6464
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.384
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prismatic
_exptl_crystal_F_000             1806
_exptl_crystal_size_max          0.551
_exptl_crystal_size_mid          0.432
_exptl_crystal_size_min          0.371
_refine_diff_density_max         1.224
_refine_diff_density_min         -2.437
_refine_diff_density_rms         0.162
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.848
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     918
_refine_ls_number_reflns         24916
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.848
_refine_ls_R_factor_all          0.2367
_refine_ls_R_factor_gt           0.0747
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1744
_refine_ls_wR_factor_ref         0.2627
_reflns_number_gt                7753
_reflns_number_total             24916
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300942p_si_003.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4079685
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zr1 Zr 0.4793(9) 0.19470(19) 0.25790(12) 0.0356(5) Uani 0.86(4) 1 d P A 1
Zr1A Zr 0.507(3) 0.1923(8) 0.2618(8) 0.017(4) Uiso 0.14(4) 1 d P A 2
Br1 Br 0.56739(10) -0.09093(5) 0.43668(4) 0.0684(3) Uani 1 1 d . A .
Br2 Br -0.07509(10) 0.32324(7) 0.07242(5) 0.0877(4) Uani 1 1 d . A .
N1 N 0.5397(6) 0.3050(3) 0.3188(2) 0.0373(15) Uani 1 1 d . . .
N2 N 0.6023(6) 0.1930(3) 0.3359(2) 0.0418(16) Uani 1 1 d . . .
N3 N 0.6124(6) 0.3074(4) 0.4061(2) 0.0447(16) Uani 1 1 d . . .
H3 H 0.5624 0.3457 0.4173 0.054 Uiso 1 1 calc R A .
N4 N 0.6410(5) 0.2139(4) 0.2052(2) 0.0402(15) Uani 1 1 d . . .
N5 N 0.4179(6) 0.2092(4) 0.1786(2) 0.0410(16) Uani 1 1 d . . .
N6 N 0.5898(6) 0.2299(4) 0.1202(2) 0.0476(18) Uani 1 1 d . . .
H6 H 0.6671 0.2598 0.1201 0.057 Uiso 1 1 calc R A .
C1 C 0.5879(7) 0.2697(4) 0.3557(3) 0.0375(18) Uani 1 1 d . A .
C2 C 0.5360(8) 0.3915(4) 0.3269(3) 0.047(2) Uani 1 1 d . A .
H2 H 0.4828 0.4102 0.3569 0.057 Uiso 1 1 calc R . .
C3 C 0.4597(11) 0.4070(5) 0.2791(3) 0.070(3) Uani 1 1 d . . .
H3A H 0.5090 0.3869 0.2493 0.105 Uiso 1 1 calc R A .
H3B H 0.4563 0.4637 0.2835 0.105 Uiso 1 1 calc R . .
H3C H 0.3655 0.3801 0.2743 0.105 Uiso 1 1 calc R . .
C4 C 0.6838(9) 0.4373(5) 0.3369(3) 0.072(3) Uani 1 1 d . . .
H4A H 0.7325 0.4248 0.3660 0.107 Uiso 1 1 calc R A .
H4B H 0.6770 0.4940 0.3439 0.107 Uiso 1 1 calc R . .
H4C H 0.7348 0.4217 0.3069 0.107 Uiso 1 1 calc R . .
C5 C 0.7140(8) 0.2902(5) 0.4435(3) 0.052(2) Uani 1 1 d . A .
H5 H 0.7194 0.2321 0.4354 0.062 Uiso 1 1 calc R . .
C6 C 0.8565(10) 0.3317(7) 0.4406(5) 0.103(4) Uani 1 1 d . . .
H6A H 0.8841 0.3158 0.4060 0.154 Uiso 1 1 calc R A .
H6B H 0.9233 0.3171 0.4641 0.154 Uiso 1 1 calc R . .
H6C H 0.8538 0.3889 0.4498 0.154 Uiso 1 1 calc R . .
C7 C 0.6661(12) 0.3151(6) 0.4970(3) 0.089(3) Uani 1 1 d . . .
H7A H 0.6586 0.3718 0.5053 0.133 Uiso 1 1 calc R A .
H7B H 0.7332 0.3031 0.5215 0.133 Uiso 1 1 calc R . .
H7C H 0.5759 0.2863 0.4983 0.133 Uiso 1 1 calc R . .
C8 C 0.5535(7) 0.2186(4) 0.1666(3) 0.0383(18) Uani 1 1 d . A .
C9 C 0.7935(7) 0.2112(5) 0.2017(3) 0.046(2) Uani 1 1 d . A .
H9 H 0.8083 0.1899 0.1652 0.056 Uiso 1 1 calc R . .
C10 C 0.8457(10) 0.1563(7) 0.2309(5) 0.109(4) Uani 1 1 d . . .
H10A H 0.8405 0.1782 0.2672 0.163 Uiso 1 1 calc R A .
H10B H 0.9417 0.1494 0.2242 0.163 Uiso 1 1 calc R . .
H10C H 0.7891 0.1052 0.2205 0.163 Uiso 1 1 calc R . .
C11 C 0.8701(9) 0.2949(5) 0.2182(5) 0.095(4) Uani 1 1 d . . .
H11A H 0.8652 0.3154 0.2546 0.143 Uiso 1 1 calc R A .
H11B H 0.8271 0.3293 0.1996 0.143 Uiso 1 1 calc R . .
H11C H 0.9669 0.2934 0.2108 0.143 Uiso 1 1 calc R . .
C12 C 0.5097(9) 0.1960(6) 0.0703(3) 0.066(3) Uani 1 1 d . A .
H12 H 0.4078 0.1865 0.0723 0.079 Uiso 1 1 calc R B 1
C13 C 0.5512(14) 0.2416(7) 0.0312(4) 0.117(5) Uani 1 1 d . . .
H13A H 0.6515 0.2454 0.0298 0.175 Uiso 1 1 calc R A .
H13B H 0.5225 0.2947 0.0407 0.175 Uiso 1 1 calc R . .
H13C H 0.5062 0.2141 -0.0022 0.175 Uiso 1 1 calc R . .
C14 C 0.583(3) 0.1162(13) 0.0482(9) 0.089(8) Uani 0.50 1 d P A 1
H14A H 0.6777 0.1309 0.0416 0.133 Uiso 0.50 1 calc PR A 1
H14B H 0.5309 0.0860 0.0167 0.133 Uiso 0.50 1 calc PR A 1
H14C H 0.5824 0.0840 0.0732 0.133 Uiso 0.50 1 calc PR A 1
C14B C 0.470(3) 0.1117(14) 0.0566(10) 0.101(9) Uani 0.50 1 d P A 2
H14G H 0.4313 0.0951 0.0854 0.121 Uiso 0.50 1 calc PR A 2
H14H H 0.5510 0.0845 0.0476 0.121 Uiso 0.50 1 calc PR A 2
H14I H 0.4004 0.0985 0.0276 0.121 Uiso 0.50 1 calc PR A 2
C21 C 0.5996(8) 0.1327(4) 0.3641(3) 0.0412(19) Uani 1 1 d . A .
C22 C 0.7044(9) 0.0806(5) 0.3582(3) 0.047(2) Uani 1 1 d . . .
H22 H 0.7800 0.0900 0.3392 0.056 Uiso 1 1 calc R A .
C23 C 0.6961(9) 0.0145(5) 0.3807(3) 0.053(2) Uani 1 1 d . A .
H23 H 0.7666 -0.0196 0.3770 0.064 Uiso 1 1 calc R . .
C24 C 0.5838(9) 0.0002(5) 0.4083(3) 0.053(2) Uani 1 1 d . . .
C25 C 0.4812(9) 0.0537(5) 0.4155(3) 0.055(2) Uani 1 1 d . A .
H25 H 0.4069 0.0453 0.4352 0.066 Uiso 1 1 calc R . .
C26 C 0.4897(7) 0.1186(4) 0.3935(3) 0.045(2) Uani 1 1 d . . .
H26 H 0.4208 0.1536 0.3984 0.054 Uiso 1 1 calc R A .
C31 C 0.3064(7) 0.2364(5) 0.1529(3) 0.044(2) Uani 1 1 d . A .
C32 C 0.3088(8) 0.3160(5) 0.1494(3) 0.055(2) Uani 1 1 d . . .
H32 H 0.3881 0.3521 0.1628 0.066 Uiso 1 1 calc R A .
C33 C 0.1966(8) 0.3419(5) 0.1264(3) 0.057(2) Uani 1 1 d . A .
H33 H 0.1985 0.3956 0.1253 0.068 Uiso 1 1 calc R . .
C34 C 0.0811(7) 0.2884(5) 0.1050(3) 0.054(2) Uani 1 1 d . . .
C35 C 0.0769(8) 0.2085(5) 0.1081(3) 0.052(2) Uani 1 1 d . A .
H35 H -0.0011 0.1722 0.0933 0.063 Uiso 1 1 calc R . .
C36 C 0.1875(8) 0.1830(5) 0.1329(3) 0.050(2) Uani 1 1 d . . .
H36 H 0.1826 0.1302 0.1362 0.060 Uiso 1 1 calc R A .
C41 C 0.4728(8) 0.0598(4) 0.2503(3) 0.045(2) Uani 1 1 d . . .
H41A H 0.5675 0.0486 0.2589 0.054 Uiso 1 1 calc R A 1
H41B H 0.4147 0.0461 0.2763 0.054 Uiso 1 1 calc R A 1
C42 C 0.4200(9) 0.0046(5) 0.1996(3) 0.052(2) Uani 1 1 d . A .
C43 C 0.5090(11) -0.0203(5) 0.1616(4) 0.078(3) Uani 1 1 d . . .
H43 H 0.6042 -0.0011 0.1679 0.094 Uiso 1 1 calc R A .
C44 C 0.4622(15) -0.0729(7) 0.1144(4) 0.100(4) Uani 1 1 d . A .
H44 H 0.5259 -0.0880 0.0899 0.121 Uiso 1 1 calc R . .
C45 C 0.3226(15) -0.1026(7) 0.1037(4) 0.100(4) Uani 1 1 d . . .
H45 H 0.2893 -0.1377 0.0723 0.120 Uiso 1 1 calc R A .
C46 C 0.2358(13) -0.0782(6) 0.1412(4) 0.085(4) Uani 1 1 d . A .
H46 H 0.1409 -0.0979 0.1353 0.102 Uiso 1 1 calc R . .
C47 C 0.2823(9) -0.0258(5) 0.1874(3) 0.068(3) Uani 1 1 d . . .
H47 H 0.2174 -0.0103 0.2114 0.081 Uiso 1 1 calc R A .
C51 C 0.2467(7) 0.1963(5) 0.2650(3) 0.054(2) Uani 1 1 d . . .
H51A H 0.2193 0.2462 0.2585 0.065 Uiso 1 1 calc R A 1
H51B H 0.1966 0.1525 0.2385 0.065 Uiso 1 1 calc R A 1
C52 C 0.2030(7) 0.1888(5) 0.3163(3) 0.045(2) Uani 1 1 d . A .
C53 C 0.2183(8) 0.2545(5) 0.3593(4) 0.059(2) Uani 1 1 d . . .
H53 H 0.2519 0.3053 0.3557 0.071 Uiso 1 1 calc R A .
C54 C 0.1843(10) 0.2443(7) 0.4065(4) 0.078(3) Uani 1 1 d . A .
H54 H 0.1990 0.2884 0.4347 0.094 Uiso 1 1 calc R . .
C55 C 0.1286(10) 0.1711(7) 0.4141(4) 0.077(3) Uani 1 1 d . . .
H55 H 0.1042 0.1660 0.4465 0.092 Uiso 1 1 calc R A .
C56 C 0.1105(8) 0.1056(7) 0.3719(4) 0.069(3) Uani 1 1 d . A .
H56 H 0.0726 0.0556 0.3758 0.083 Uiso 1 1 calc R . .
C57 C 0.1489(8) 0.1142(5) 0.3240(3) 0.059(2) Uani 1 1 d . . .
H57 H 0.1384 0.0694 0.2962 0.071 Uiso 1 1 calc R A .
Zr2 Zr 0.96689(7) 0.68435(4) 0.25742(3) 0.0386(2) Uani 1 1 d . . .
Br3 Br 0.66174(11) 0.55160(6) 0.48914(4) 0.0828(4) Uani 1 1 d . . .
Br4 Br 1.30663(10) 0.53632(6) -0.00714(4) 0.0745(3) Uani 1 1 d . . .
N1A N 1.1386(6) 0.7660(3) 0.3063(2) 0.0395(16) Uani 1 1 d . . .
N2A N 0.9515(5) 0.7299(3) 0.3450(2) 0.0375(15) Uani 1 1 d . . .
N3A N 1.1505(6) 0.8057(3) 0.3993(2) 0.0447(17) Uani 1 1 d . . .
H3A1 H 1.2410 0.8098 0.4018 0.054 Uiso 1 1 calc R . .
N4A N 0.8719(7) 0.7738(4) 0.2221(2) 0.0489(17) Uani 1 1 d . . .
N5A N 0.9703(7) 0.6778(4) 0.1711(2) 0.0471(17) Uani 1 1 d . . .
N6A N 0.8572(8) 0.7700(4) 0.1329(2) 0.063(2) Uani 1 1 d . . .
H6A1 H 0.8557 0.8211 0.1378 0.076 Uiso 1 1 calc R . .
C1A C 1.0844(7) 0.7677(4) 0.3516(3) 0.0389(18) Uani 1 1 d . . .
C2A C 1.2699(7) 0.8156(4) 0.3028(3) 0.047(2) Uani 1 1 d . . .
H2A H 1.3451 0.8060 0.3264 0.056 Uiso 1 1 calc R . .
C3A C 1.2502(10) 0.9040(4) 0.3149(3) 0.063(3) Uani 1 1 d . . .
H3D H 1.1810 0.9135 0.2901 0.094 Uiso 1 1 calc R . .
H3E H 1.3380 0.9350 0.3134 0.094 Uiso 1 1 calc R . .
H3F H 1.2189 0.9196 0.3490 0.094 Uiso 1 1 calc R . .
C4A C 1.3073(9) 0.7899(6) 0.2471(3) 0.073(3) Uani 1 1 d . . .
H4D H 1.3238 0.7344 0.2395 0.110 Uiso 1 1 calc R . .
H4E H 1.3908 0.8223 0.2425 0.110 Uiso 1 1 calc R . .
H4F H 1.2309 0.7968 0.2241 0.110 Uiso 1 1 calc R . .
C5A C 1.0843(8) 0.8396(4) 0.4459(3) 0.043(2) Uani 1 1 d . . .
H5A H 1.0309 0.7958 0.4569 0.051 Uiso 1 1 calc R . .
C6A C 1.1936(10) 0.8814(5) 0.4885(3) 0.072(3) Uani 1 1 d . . .
H6D H 1.2599 0.8450 0.4937 0.108 Uiso 1 1 calc R . .
H6E H 1.1490 0.8991 0.5198 0.108 Uiso 1 1 calc R . .
H6F H 1.2419 0.9271 0.4794 0.108 Uiso 1 1 calc R . .
C7A C 0.9847(10) 0.8969(6) 0.4352(3) 0.072(3) Uani 1 1 d . . .
H7D H 1.0359 0.9405 0.4248 0.108 Uiso 1 1 calc R . .
H7E H 0.9393 0.9175 0.4659 0.108 Uiso 1 1 calc R . .
H7F H 0.9149 0.8693 0.4079 0.108 Uiso 1 1 calc R . .
C8A C 0.9001(8) 0.7417(5) 0.1737(3) 0.043(2) Uani 1 1 d . . .
C9A C 0.7781(10) 0.8358(5) 0.2348(3) 0.058(2) Uani 1 1 d . . .
H9A H 0.7037 0.8274 0.2066 0.070 Uiso 1 1 calc R . .
C10A C 0.8597(13) 0.9186(5) 0.2411(4) 0.092(4) Uani 1 1 d . . .
H10D H 0.9254 0.9299 0.2712 0.139 Uiso 1 1 calc R . .
H10E H 0.7952 0.9586 0.2450 0.139 Uiso 1 1 calc R . .
H10F H 0.9099 0.9193 0.2110 0.139 Uiso 1 1 calc R . .
C11A C 0.7115(10) 0.8282(5) 0.2836(3) 0.070(3) Uani 1 1 d . . .
H11D H 0.6616 0.7755 0.2785 0.105 Uiso 1 1 calc R . .
H11E H 0.6471 0.8678 0.2919 0.105 Uiso 1 1 calc R . .
H11F H 0.7836 0.8365 0.3116 0.105 Uiso 1 1 calc R . .
C12A C 0.8122(10) 0.7194(6) 0.0800(3) 0.074(3) Uani 1 1 d . . .
H12A H 0.8679 0.6738 0.0721 0.089 Uiso 1 1 calc R . .
C13A C 0.8346(13) 0.7716(9) 0.0421(4) 0.128(5) Uani 1 1 d . . .
H13D H 0.7816 0.8168 0.0508 0.192 Uiso 1 1 calc R . .
H13E H 0.8035 0.7408 0.0078 0.192 Uiso 1 1 calc R . .
H13F H 0.9329 0.7904 0.0437 0.192 Uiso 1 1 calc R . .
C14A C 0.6606(11) 0.6902(6) 0.0775(4) 0.091(4) Uani 1 1 d . . .
H14D H 0.6453 0.6605 0.1034 0.137 Uiso 1 1 calc R . .
H14E H 0.6316 0.6559 0.0439 0.137 Uiso 1 1 calc R . .
H14F H 0.6067 0.7352 0.0834 0.137 Uiso 1 1 calc R . .
C21A C 0.8929(7) 0.6925(4) 0.3828(3) 0.0345(17) Uani 1 1 d . . .
C22A C 0.7546(7) 0.7067(4) 0.3956(3) 0.045(2) Uani 1 1 d . . .
H22A H 0.7074 0.7431 0.3820 0.054 Uiso 1 1 calc R . .
C23A C 0.6910(9) 0.6657(5) 0.4285(3) 0.061(3) Uani 1 1 d . . .
H23A H 0.6004 0.6749 0.4372 0.073 Uiso 1 1 calc R . .
C24A C 0.7584(9) 0.6125(5) 0.4482(3) 0.051(2) Uani 1 1 d . . .
C25A C 0.8926(9) 0.5983(4) 0.4360(3) 0.055(2) Uani 1 1 d . . .
H25A H 0.9383 0.5620 0.4501 0.066 Uiso 1 1 calc R . .
C26A C 0.9602(8) 0.6379(4) 0.4030(3) 0.043(2) Uani 1 1 d . . .
H26A H 1.0506 0.6276 0.3945 0.051 Uiso 1 1 calc R . .
C31A C 1.0505(7) 0.6450(4) 0.1295(3) 0.0392(18) Uani 1 1 d . . .
C32A C 1.1504(8) 0.6936(5) 0.1131(3) 0.052(2) Uani 1 1 d . . .
H32A H 1.1657 0.7481 0.1293 0.062 Uiso 1 1 calc R . .
C33A C 1.2294(8) 0.6626(5) 0.0724(3) 0.052(2) Uani 1 1 d . . .
H33A H 1.2966 0.6958 0.0610 0.063 Uiso 1 1 calc R . .
C34A C 1.2052(8) 0.5800(5) 0.0489(3) 0.050(2) Uani 1 1 d . . .
C35A C 1.1031(8) 0.5310(5) 0.0652(3) 0.052(2) Uani 1 1 d . . .
H35A H 1.0863 0.4765 0.0492 0.062 Uiso 1 1 calc R . .
C36A C 1.0260(7) 0.5642(4) 0.1057(3) 0.0407(19) Uani 1 1 d . . .
H36A H 0.9572 0.5316 0.1168 0.049 Uiso 1 1 calc R . .
C51A C 1.1043(7) 0.5833(4) 0.2368(3) 0.045(2) Uani 1 1 d . . .
H51C H 1.0525 0.5391 0.2110 0.055 Uiso 1 1 calc R . .
H51D H 1.1870 0.6022 0.2217 0.055 Uiso 1 1 calc R . .
C52A C 1.1496(8) 0.5538(4) 0.2832(3) 0.0448(19) Uani 1 1 d . . .
C53A C 1.0760(9) 0.4882(5) 0.2959(3) 0.057(2) Uani 1 1 d . . .
H53A H 0.9995 0.4603 0.2738 0.068 Uiso 1 1 calc R . .
C54A C 1.1124(11) 0.4627(6) 0.3406(4) 0.073(3) Uani 1 1 d . . .
H54A H 1.0597 0.4193 0.3484 0.088 Uiso 1 1 calc R . .
C55A C 1.2255(12) 0.5019(7) 0.3721(4) 0.083(3) Uani 1 1 d . . .
H55A H 1.2531 0.4844 0.4013 0.100 Uiso 1 1 calc R . .
C56A C 1.3007(10) 0.5685(6) 0.3613(4) 0.066(3) Uani 1 1 d . . .
H56A H 1.3752 0.5969 0.3843 0.079 Uiso 1 1 calc R . .
C57A C 1.2667(8) 0.5923(5) 0.3178(3) 0.053(2) Uani 1 1 d . . .
H57A H 1.3217 0.6352 0.3104 0.064 Uiso 1 1 calc R . .
C41A C 0.7678(8) 0.6056(4) 0.2682(3) 0.048(2) Uani 1 1 d . . .
H41C H 0.7955 0.5645 0.2850 0.058 Uiso 1 1 calc R . .
H41D H 0.7098 0.6387 0.2908 0.058 Uiso 1 1 calc R . .
C42A C 0.6821(8) 0.5659(4) 0.2185(3) 0.043(2) Uani 1 1 d . . .
C43A C 0.7149(8) 0.4974(5) 0.1851(3) 0.051(2) Uani 1 1 d . . .
H43A H 0.7945 0.4740 0.1928 0.061 Uiso 1 1 calc R . .
C44A C 0.6296(9) 0.4632(5) 0.1399(3) 0.060(3) Uani 1 1 d . . .
H44A H 0.6521 0.4163 0.1181 0.072 Uiso 1 1 calc R . .
C45A C 0.5124(9) 0.4971(6) 0.1266(3) 0.065(3) Uani 1 1 d . . .
H45A H 0.4570 0.4751 0.0958 0.078 Uiso 1 1 calc R . .
C46A C 0.4817(10) 0.5628(6) 0.1597(4) 0.068(3) Uani 1 1 d . . .
H46A H 0.4017 0.5862 0.1524 0.081 Uiso 1 1 calc R . .
C47A C 0.5657(8) 0.5967(4) 0.2045(3) 0.057(2) Uani 1 1 d . . .
H47A H 0.5412 0.6431 0.2261 0.068 Uiso 1 1 calc R . .
C64 C 0.0704(8) -0.0055(4) 0.0393(3) 0.077(5) Uiso 0.50 1 d PR . .
C63 C 0.1396(8) 0.0065(4) -0.0295(3) 0.167(12) Uiso 0.50 1 d PR . .
C61 C 0.0451(8) 0.0010(4) -0.0715(3) 0.217(19) Uiso 0.50 1 d PR . .
C62 C 0.0201(8) 0.0002(4) -0.0453(3) 0.47(3) Uiso 1 1 d R . .
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -2.9673 0.5597 '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
N1 Zr1 N4 98.0(3) . .
N1 Zr1 N5 117.2(3) . .
N4 Zr1 N5 59.4(2) . .
N1 Zr1 C51 94.7(4) . .
N4 Zr1 C51 140.9(4) . .
N5 Zr1 C51 82.0(4) . .
N1 Zr1 C41 136.9(4) . .
N4 Zr1 C41 101.0(4) . .
N5 Zr1 C41 105.7(2) . .
C51 Zr1 C41 94.3(3) . .
N1 Zr1 N2 58.2(2) . .
N4 Zr1 N2 105.8(4) . .
N5 Zr1 N2 164.8(4) . .
C51 Zr1 N2 112.3(3) . .
C41 Zr1 N2 79.5(3) . .
N1 Zr1 C8 109.7(2) . .
N4 Zr1 C8 29.0(2) . .
N5 Zr1 C8 30.3(2) . .
C51 Zr1 C8 112.1(4) . .
C41 Zr1 C8 105.5(3) . .
N2 Zr1 C8 134.8(4) . .
N1 Zr1 C1 29.5(2) . .
N4 Zr1 C1 107.3(3) . .
N5 Zr1 C1 146.1(2) . .
C51 Zr1 C1 101.8(3) . .
C41 Zr1 C1 107.5(3) . .
N2 Zr1 C1 29.1(2) . .
C8 Zr1 C1 129.9(2) . .
N4 Zr1A N2 117.5(15) . .
N4 Zr1A N1 102.2(7) . .
N2 Zr1A N1 62.1(7) . .
N4 Zr1A C41 105.9(7) . .
N2 Zr1A C41 85.6(8) . .
N1 Zr1A C41 144.5(11) . .
N4 Zr1A N5 57.6(5) . .
N2 Zr1A N5 172.0(8) . .
N1 Zr1A N5 111.6(9) . .
C41 Zr1A N5 101.7(9) . .
N4 Zr1A C51 130.5(14) . .
N2 Zr1A C51 110.4(6) . .
N1 Zr1A C51 88.9(7) . .
C41 Zr1A C51 89.1(8) . .
N5 Zr1A C51 73.4(10) . .
N4 Zr1A C1 115.5(11) . .
N2 Zr1A C1 30.8(4) . .
N1 Zr1A C1 31.5(4) . .
C41 Zr1A C1 114.4(10) . .
N5 Zr1A C1 143.1(7) . .
C51 Zr1A C1 99.0(5) . .
N4 Zr1A C8 27.8(4) . .
N2 Zr1A C8 145.0(12) . .
N1 Zr1A C8 109.4(5) . .
C41 Zr1A C8 105.6(6) . .
N5 Zr1A C8 29.8(3) . .
C51 Zr1A C8 102.9(12) . .
C1 Zr1A C8 134.2(6) . .
C1 N1 C2 123.5(6) . .
C1 N1 Zr1A 92.1(8) . .
C2 N1 Zr1A 144.2(8) . .
C1 N1 Zr1 97.4(5) . .
C2 N1 Zr1 139.1(5) . .
Zr1A N1 Zr1 7.5(7) . .
C1 N2 C21 124.9(6) . .
C1 N2 Zr1A 94.2(6) . .
C21 N2 Zr1A 131.1(5) . .
C1 N2 Zr1 91.8(5) . .
C21 N2 Zr1 130.3(4) . .
Zr1A N2 Zr1 5.0(5) . .
C1 N3 C5 127.0(7) . .
C8 N4 C9 123.5(6) . .
C8 N4 Zr1A 103.6(10) . .
C9 N4 Zr1A 132.1(10) . .
C8 N4 Zr1 96.4(4) . .
C9 N4 Zr1 139.3(5) . .
Zr1A N4 Zr1 7.3(7) . .
C8 N5 C31 122.9(6) . .
C8 N5 Zr1 93.4(5) . .
C31 N5 Zr1 138.4(5) . .
C8 N5 Zr1A 88.1(7) . .
C31 N5 Zr1A 143.6(7) . .
Zr1 N5 Zr1A 5.5(4) . .
C8 N6 C12 126.0(5) . .
N2 C1 N3 125.1(7) . .
N2 C1 N1 111.0(6) . .
N3 C1 N1 123.8(7) . .
N2 C1 Zr1A 55.0(6) . .
N3 C1 Zr1A 172.3(7) . .
N1 C1 Zr1A 56.4(6) . .
N2 C1 Zr1 59.0(4) . .
N3 C1 Zr1 167.7(5) . .
N1 C1 Zr1 53.2(4) . .
Zr1A C1 Zr1 5.4(5) . .
N1 C2 C3 107.9(6) . .
N1 C2 C4 111.9(7) . .
C3 C2 C4 110.3(6) . .
N3 C5 C6 110.7(7) . .
N3 C5 C7 109.9(7) . .
C6 C5 C7 110.9(8) . .
N4 C8 N6 125.9(6) . .
N4 C8 N5 110.8(6) . .
N6 C8 N5 123.3(7) . .
N4 C8 Zr1 54.5(4) . .
N6 C8 Zr1 179.3(5) . .
N5 C8 Zr1 56.2(4) . .
N4 C8 Zr1A 48.6(8) . .
N6 C8 Zr1A 174.3(9) . .
N5 C8 Zr1A 62.2(8) . .
Zr1 C8 Zr1A 6.0(5) . .
C10 C9 N4 110.6(6) . .
C10 C9 C11 113.1(8) . .
N4 C9 C11 110.2(7) . .
C14B C12 N6 117.5(13) . .
C14B C12 C13 121.9(13) . .
N6 C12 C13 111.2(6) . .
C14B C12 C14 42.6(11) . .
N6 C12 C14 102.7(12) . .
C13 C12 C14 98.4(11) . .
C26 C21 C22 118.8(7) . .
C26 C21 N2 122.1(8) . .
C22 C21 N2 118.9(6) . .
C21 C22 C23 120.4(7) . .
C24 C23 C22 119.8(9) . .
C23 C24 C25 119.7(7) . .
C23 C24 Br1 120.4(8) . .
C25 C24 Br1 120.0(6) . .
C26 C25 C24 120.4(8) . .
C25 C26 C21 120.9(9) . .
C36 C31 C32 119.1(7) . .
C36 C31 N5 118.8(7) . .
C32 C31 N5 122.0(6) . .
C33 C32 C31 121.0(7) . .
C32 C33 C34 119.8(8) . .
C33 C34 C35 119.9(7) . .
C33 C34 Br2 120.4(6) . .
C35 C34 Br2 119.7(5) . .
C36 C35 C34 120.3(6) . .
C35 C36 C31 119.7(7) . .
C42 C41 Zr1A 122.8(9) . .
C42 C41 Zr1 118.4(5) . .
Zr1A C41 Zr1 7.2(7) . .
C47 C42 C43 115.1(8) . .
C47 C42 C41 123.1(8) . .
C43 C42 C41 121.9(8) . .
C42 C43 C44 122.7(10) . .
C45 C44 C43 120.5(11) . .
C46 C45 C44 116.6(10) . .
C45 C46 C47 122.7(10) . .
C42 C47 C46 122.5(10) . .
C52 C51 Zr1 113.7(5) . .
C52 C51 Zr1A 110.5(7) . .
Zr1 C51 Zr1A 3.2(5) . .
C57 C52 C53 117.2(7) . .
C57 C52 C51 120.8(7) . .
C53 C52 C51 122.0(6) . .
C54 C53 C52 120.3(8) . .
C53 C54 C55 122.7(9) . .
C54 C55 C56 117.9(9) . .
C55 C56 C57 120.2(9) . .
C56 C57 C52 121.7(8) . .
N1A Zr2 N4A 98.0(2) . .
N1A Zr2 C51A 92.8(2) . .
N4A Zr2 C51A 139.7(3) . .
N1A Zr2 N5A 114.63(19) . .
N4A Zr2 N5A 58.7(3) . .
C51A Zr2 N5A 81.4(3) . .
N1A Zr2 C41A 138.0(2) . .
N4A Zr2 C41A 100.7(3) . .
C51A Zr2 C41A 96.6(3) . .
N5A Zr2 C41A 107.3(2) . .
N1A Zr2 N2A 59.26(18) . .
N4A Zr2 N2A 104.9(2) . .
C51A Zr2 N2A 113.9(2) . .
N5A Zr2 N2A 162.8(2) . .
C41A Zr2 N2A 79.6(2) . .
N1A Zr2 C1A 29.42(18) . .
N4A Zr2 C1A 105.5(2) . .
C51A Zr2 C1A 102.8(2) . .
N5A Zr2 C1A 142.90(18) . .
C41A Zr2 C1A 108.8(2) . .
N2A Zr2 C1A 30.02(18) . .
N1A Zr2 C8A 109.1(2) . .
N4A Zr2 C8A 29.3(2) . .
C51A Zr2 C8A 110.7(3) . .
N5A Zr2 C8A 29.4(2) . .
C41A Zr2 C8A 105.5(2) . .
N2A Zr2 C8A 134.1(2) . .
C1A Zr2 C8A 128.1(2) . .
C1A N1A C2A 121.6(5) . .
C1A N1A Zr2 96.8(3) . .
C2A N1A Zr2 141.4(4) . .
C1A N2A C21A 122.3(6) . .
C1A N2A Zr2 91.7(4) . .
C21A N2A Zr2 132.3(4) . .
C1A N3A C5A 127.2(6) . .
C8A N4A C9A 123.1(7) . .
C8A N4A Zr2 96.1(5) . .
C9A N4A Zr2 139.2(5) . .
C8A N5A C31A 125.0(6) . .
C8A N5A Zr2 93.3(5) . .
C31A N5A Zr2 138.3(5) . .
C8A N6A C12A 124.9(7) . .
N1A C1A N2A 111.6(6) . .
N1A C1A N3A 125.3(5) . .
N2A C1A N3A 123.1(6) . .
N1A C1A Zr2 53.7(3) . .
N2A C1A Zr2 58.3(3) . .
N3A C1A Zr2 175.8(6) . .
N1A C2A C3A 111.2(7) . .
N1A C2A C4A 106.3(5) . .
C3A C2A C4A 109.0(7) . .
N3A C5A C7A 110.2(7) . .
N3A C5A C6A 110.5(6) . .
C7A C5A C6A 110.3(7) . .
N5A C8A N4A 111.8(7) . .
N5A C8A N6A 125.2(8) . .
N4A C8A N6A 123.0(8) . .
N5A C8A Zr2 57.3(4) . .
N4A C8A Zr2 54.5(4) . .
N6A C8A Zr2 175.9(6) . .
N4A C9A C11A 108.7(7) . .
N4A C9A C10A 109.9(7) . .
C11A C9A C10A 111.6(7) . .
C14A C12A N6A 108.9(8) . .
C14A C12A C13A 109.5(9) . .
N6A C12A C13A 107.8(9) . .
C26A C21A C22A 119.6(6) . .
C26A C21A N2A 122.4(6) . .
C22A C21A N2A 117.7(7) . .
C23A C22A C21A 118.8(8) . .
C24A C23A C22A 121.0(8) . .
C23A C24A C25A 120.5(7) . .
C23A C24A Br3 119.5(6) . .
C25A C24A Br3 119.8(7) . .
C24A C25A C26A 120.4(8) . .
C21A C26A C25A 119.6(7) . .
C32A C31A C36A 120.2(7) . .
C32A C31A N5A 120.0(7) . .
C36A C31A N5A 119.7(6) . .
C31A C32A C33A 120.8(7) . .
C32A C33A C34A 118.6(6) . .
C35A C34A C33A 120.5(7) . .
C35A C34A Br4 119.6(6) . .
C33A C34A Br4 119.8(5) . .
C34A C35A C36A 119.3(7) . .
C31A C36A C35A 120.6(6) . .
C52A C51A Zr2 111.7(5) . .
C53A C52A C57A 115.8(7) . .
C53A C52A C51A 121.9(6) . .
C57A C52A C51A 122.3(6) . .
C52A C53A C54A 122.6(8) . .
C55A C54A C53A 118.9(8) . .
C54A C55A C56A 120.4(9) . .
C57A C56A C55A 120.6(8) . .
C56A C57A C52A 121.7(7) . .
C42A C41A Zr2 113.5(4) . .
C47A C42A C43A 116.4(7) . .
C47A C42A C41A 120.2(8) . .
C43A C42A C41A 123.4(8) . .
C42A C43A C44A 120.4(9) . .
C45A C44A C43A 121.5(9) . .
C46A C45A C44A 117.2(8) . .
C45A C46A C47A 121.4(10) . .
C42A C47A C46A 123.1(8) . .
C62 C64 C61 26.9(5) 2 2
C62 C64 C63 17.4(5) 2 2
C61 C64 C63 43.3(4) 2 2
C62 C64 C63 119.8(10) 2 .
C61 C64 C63 146.5(6) 2 .
C63 C64 C63 104.5(4) 2 .
C62 C63 C61 33.2 . .
C62 C63 C64 13.1(4) . 2
C61 C63 C64 45.7(4) . 2
C62 C63 C64 87.3 . .
C61 C63 C64 120.4 . .
C64 C63 C64 75.5(4) 2 .
C62 C61 C63 59.0 . .
C62 C61 C64 32.7(6) . 2
C63 C61 C64 91.1(6) . 2
C61 C62 C64 120.4(10) . 2
C61 C62 C63 87.8 . .
C64 C62 C63 149.5(9) 2 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zr1 N1 2.197(6) .
Zr1 N4 2.202(7) .
Zr1 N5 2.238(8) .
Zr1 C51 2.248(12) .
Zr1 C41 2.276(8) .
Zr1 N2 2.335(9) .
Zr1 C8 2.687(7) .
Zr1 C1 2.723(8) .
Zr1A N4 2.112(14) .
Zr1A N2 2.12(3) .
Zr1A N1 2.154(16) .
Zr1A C41 2.217(14) .
Zr1A N5 2.42(3) .
Zr1A C51 2.50(3) .
Zr1A C1 2.58(2) .
Zr1A C8 2.736(18) .
Br1 C24 1.890(7) .
Br2 C34 1.899(8) .
N1 C1 1.351(9) .
N1 C2 1.458(9) .
N2 C1 1.327(9) .
N2 C21 1.415(9) .
N3 C1 1.346(9) .
N3 C5 1.451(10) .
N4 C8 1.312(9) .
N4 C9 1.473(8) .
N5 C8 1.359(8) .
N5 C31 1.408(9) .
N6 C8 1.356(8) .
N6 C12 1.460(9) .
C2 C3 1.522(11) .
C2 C4 1.529(9) .
C5 C6 1.492(11) .
C5 C7 1.503(11) .
C9 C10 1.462(13) .
C9 C11 1.507(10) .
C12 C14B 1.42(2) .
C12 C13 1.493(12) .
C12 C14 1.61(3) .
C21 C26 1.384(9) .
C21 C22 1.399(11) .
C22 C23 1.402(10) .
C23 C24 1.371(11) .
C24 C25 1.402(12) .
C25 C26 1.374(10) .
C31 C36 1.387(8) .
C31 C32 1.393(11) .
C32 C33 1.367(11) .
C33 C34 1.371(9) .
C34 C35 1.393(11) .
C35 C36 1.374(11) .
C41 C42 1.489(10) .
C42 C47 1.362(10) .
C42 C43 1.382(12) .
C43 C44 1.391(13) .
C44 C45 1.372(15) .
C45 C46 1.356(15) .
C46 C47 1.370(12) .
C51 C52 1.485(10) .
C52 C57 1.400(9) .
C52 C53 1.402(11) .
C53 C54 1.363(11) .
C54 C55 1.383(13) .
C55 C56 1.386(13) .
C56 C57 1.388(11) .
Zr2 N1A 2.197(5) .
Zr2 N4A 2.218(7) .
Zr2 C51A 2.267(8) .
Zr2 N5A 2.282(6) .
Zr2 C41A 2.301(6) .
Zr2 N2A 2.304(5) .
Zr2 C1A 2.706(7) .
Zr2 C8A 2.708(8) .
Br3 C24A 1.900(7) .
Br4 C34A 1.879(8) .
N1A C1A 1.339(8) .
N1A C2A 1.471(7) .
N2A C1A 1.354(7) .
N2A C21A 1.430(8) .
N3A C1A 1.373(8) .
N3A C5A 1.456(9) .
N4A C8A 1.335(9) .
N4A C9A 1.454(11) .
N5A C8A 1.332(10) .
N5A C31A 1.426(9) .
N6A C8A 1.350(10) .
N6A C12A 1.490(10) .
C2A C3A 1.512(11) .
C2A C4A 1.523(10) .
C5A C7A 1.496(12) .
C5A C6A 1.497(10) .
C9A C11A 1.509(11) .
C9A C10A 1.525(11) .
C12A C14A 1.482(13) .
C12A C13A 1.510(14) .
C21A C26A 1.376(10) .
C21A C22A 1.417(10) .
C22A C23A 1.379(10) .
C23A C24A 1.351(12) .
C24A C25A 1.374(12) .
C25A C26A 1.384(9) .
C31A C32A 1.368(8) .
C31A C36A 1.379(9) .
C32A C33A 1.395(11) .
C33A C34A 1.404(10) .
C34A C35A 1.385(9) .
C35A C36A 1.388(10) .
C51A C52A 1.501(10) .
C52A C53A 1.390(9) .
C52A C57A 1.414(10) .
C53A C54A 1.399(12) .
C54A C55A 1.351(13) .
C55A C56A 1.390(13) .
C56A C57A 1.349(12) .
C41A C42A 1.496(9) .
C42A C47A 1.348(11) .
C42A C43A 1.379(11) .
C43A C44A 1.388(11) .
C44A C45A 1.378(13) .
C45A C46A 1.334(12) .
C46A C47A 1.373(11) .
C64 C62 0.900(15) 2
C64 C61 1.438(15) 2
C64 C63 2.010(15) 2
C64 C63 2.0348 .
C63 C62 1.1819 .
C63 C61 1.3776 .
C63 C64 2.010(15) 2
C61 C62 0.7546 .
C61 C64 1.438(15) 2
C62 C64 0.900(15) 2
