#------------------------------------------------------------------------------
#$Date: 2021-09-06 12:37:54 +0300 (Mon, 06 Sep 2021) $
#$Revision: 268598 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/84/7128432.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_7128432
loop_
_publ_author_name
'Chen, Yangxin'
'Zhu, Tingting'
'Xiong, Zheyao'
'Zhou, Yang'
'Li, Yanqiang'
'Ding, Qingran'
'Liu, Youchao'
'Chen, Xin'
'Zhao, Sangen'
'Luo, Junhua'
_publ_section_title
;
 An organic-inorganic hybrid birefringent material with diverse functional
 groups.
;
_journal_issue                   54
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              6668
_journal_page_last               6671
_journal_paper_doi               10.1039/d1cc02548a
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         '2(C2 F2 O4 Sb), 2(C H7 N4), H2 O'
_chemical_formula_sum            'C6 H16 F4 N8 O9 Sb2'
_chemical_formula_weight         663.77
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2021-01-26
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2021-03-24 deposited with the CCDC.	2021-06-03 downloaded from the CCDC.
;
_cell_angle_alpha                115.937(2)
_cell_angle_beta                 108.831(2)
_cell_angle_gamma                95.796(3)
_cell_formula_units_Z            2
_cell_length_a                   9.5230(7)
_cell_length_b                   10.6568(8)
_cell_length_c                   10.7489(8)
_cell_measurement_reflns_used    9894
_cell_measurement_temperature    200.15
_cell_measurement_theta_max      27.53
_cell_measurement_theta_min      2.31
_cell_volume                     890.09(12)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      200.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0350
_diffrn_reflns_av_unetI/netI     0.0197
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            30485
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.539
_diffrn_reflns_theta_min         2.357
_exptl_absorpt_coefficient_mu    3.140
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.477
_exptl_crystal_description       slice
_exptl_crystal_F_000             636
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.856
_refine_diff_density_min         -0.940
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.183
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     278
_refine_ls_number_reflns         4086
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.214
_refine_ls_R_factor_all          0.0231
_refine_ls_R_factor_gt           0.0206
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0106P)²+0.9705P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0418
_refine_ls_wR_factor_ref         0.0427
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3816
_reflns_number_total             4086
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1cc02548a2.cif
_cod_data_source_block           1
_cod_depositor_comments          'Adding full bibliography for 7128432.cif.'
_cod_database_code               7128432
_shelx_shelxl_version_number     2018/3
_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   0.859
_shelx_estimated_absorpt_t_min   0.834
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 N2_$1-C5_$1
 1.35 with sigma of 0.02
 N5_$1-C6_$1
 1.5 with sigma of 0.02
 N5_$3-C6_$3
 1.34 with sigma of 0.02
 N2_$2-C5_$2
 1.5 with sigma of 0.02
 N6_$3-C6_$3
 1.5 with sigma of 0.02
 N1_$2-C5_$2
 1.34 with sigma of 0.02
3.a Free rotating group:
 O9(H9A,H9B)
3.b Rotating group:
 N8(H8A,H8B), N4(H4A)
3.c Aromatic/amide H refined with riding coordinates:
 N7(H7), N3(H3)
3.d X=CH2 refined with riding coordinates:
 N5(H5A,H5B), N6(H6A,H6B), N1(H1A,H1B)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_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_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
Sb1 Sb 0.52963(2) 0.69430(2) 0.33801(2) 0.01424(5) Uani 1 1 d . . . . .
Sb2 Sb 1.00422(2) 0.31487(2) 0.67720(2) 0.01421(5) Uani 1 1 d . . . . .
F003 F 0.91393(18) 0.39159(17) 0.53932(17) 0.0255(3) Uani 1 1 d . . . . .
F004 F 0.68689(18) 0.65191(17) 0.47720(17) 0.0265(3) Uani 1 1 d . . . . .
F005 F 0.70491(16) 0.79948(17) 0.33705(18) 0.0230(3) Uani 1 1 d . . . . .
F006 F 0.79473(17) 0.22517(18) 0.62676(19) 0.0269(4) Uani 1 1 d . . . . .
O7 O 0.9577(2) 0.13079(19) 0.44714(19) 0.0187(4) Uani 1 1 d . . . . .
O2 O 0.5880(2) 0.88840(19) 0.56236(19) 0.0194(4) Uani 1 1 d . . . . .
O3 O 0.5907(2) 0.4978(2) 0.1700(2) 0.0225(4) Uani 1 1 d . . . . .
N5 N 0.8062(3) 0.3180(3) 0.2265(3) 0.0240(5) Uani 1 1 d . . . . .
H5A H 0.731582 0.349965 0.187975 0.029 Uiso 1 1 calc R U . . .
H5B H 0.846415 0.349352 0.324496 0.029 Uiso 1 1 calc R U . . .
O8 O 0.9812(2) -0.08897(19) 0.31317(19) 0.0185(4) Uani 1 1 d . . . . .
O4 O 0.5790(2) 0.3552(2) -0.0606(2) 0.0252(4) Uani 1 1 d . . . . .
O6 O 0.9350(2) 0.5103(2) 0.8326(2) 0.0234(4) Uani 1 1 d . . . . .
O5 O 0.9380(2) 0.6563(2) 1.0582(2) 0.0241(4) Uani 1 1 d . . . . .
O1 O 0.5492(2) 1.10082(19) 0.69332(19) 0.0185(4) Uani 1 1 d . . . . .
O9 O 0.6136(2) 0.3982(2) 0.4849(2) 0.0313(5) Uani 1 1 d G . . . .
H9A H 0.705935 0.388201 0.516715 0.047 Uiso 1 1 d G U . . .
H9B H 0.627500 0.475434 0.476377 0.047 Uiso 1 1 d G U . . .
N6 N 0.9697(2) 0.1726(3) 0.1936(2) 0.0230(5) Uani 1 1 d . . . . .
H6A H 1.003002 0.108478 0.133500 0.028 Uiso 1 1 calc R U . . .
H6B H 1.010242 0.203573 0.291590 0.028 Uiso 1 1 calc R U . . .
N2 N 0.4576(3) 0.1608(3) 0.1759(3) 0.0239(5) Uani 1 1 d . . . . .
H2A H 0.503(4) 0.213(4) 0.278(4) 0.029 Uiso 1 1 d . U . . .
N1 N 0.2972(3) 0.3087(3) 0.2023(3) 0.0326(6) Uani 1 1 d . . . . .
H1A H 0.224791 0.341677 0.162193 0.039 Uiso 1 1 calc R U . . .
H1B H 0.335272 0.340685 0.300490 0.039 Uiso 1 1 calc R U . . .
N8 N 0.8534(2) 0.0744(2) -0.1065(2) 0.0208(5) Uani 1 1 d . . . . .
H8A H 0.907858 0.034865 -0.057994 0.025 Uiso 1 1 d R U . . .
H8B H 0.774966 0.005111 -0.189381 0.025 Uiso 1 1 d R U . . .
N7 N 0.7975(2) 0.1753(3) -0.0113(2) 0.0216(5) Uani 1 1 d . . . . .
H7 H 0.722610 0.206949 -0.049849 0.026 Uiso 1 1 calc R U . . .
N4 N 0.3516(3) 0.0632(3) -0.1235(3) 0.0249(5) Uani 1 1 d . . . . .
H4A H 0.275153 -0.010888 -0.204032 0.030 Uiso 1 1 d R U . . .
N3 N 0.2915(3) 0.1630(3) -0.0331(3) 0.0259(5) Uani 1 1 d . . . . .
H3 H 0.216625 0.193297 -0.074056 0.031 Uiso 1 1 calc R U . . .
C6 C 0.8583(3) 0.2225(3) 0.1365(3) 0.0181(5) Uani 1 1 d . . . . .
C1 C 0.5387(3) 0.9981(3) 0.5738(3) 0.0146(5) Uani 1 1 d . . . . .
C4 C 0.9833(3) 0.0112(3) 0.4311(3) 0.0146(5) Uani 1 1 d . . . . .
C5 C 0.3492(3) 0.2108(3) 0.1147(3) 0.0223(5) Uani 1 1 d . . . . .
C3 C 0.9634(3) 0.5476(3) 0.9688(3) 0.0181(5) Uani 1 1 d . . . . .
C2 C 0.5486(3) 0.4575(3) 0.0308(3) 0.0177(5) Uani 1 1 d . . . . .
H2B H 0.493(3) 0.099(3) 0.118(4) 0.025(8) Uiso 1 1 d . . . . .
H4B H 0.385(4) 0.103(4) -0.160(4) 0.039(10) Uiso 1 1 d . . . . .
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'
F F 0.0171 0.0103 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 '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
_geom_angle_publ_flag
F004 Sb1 O2 78.17(6) . . ?
F004 Sb1 O3 76.96(6) . . ?
F004 Sb1 O1 142.44(6) . 2_676 ?
F005 Sb1 F004 84.78(7) . . ?
F005 Sb1 O2 85.43(7) . . ?
F005 Sb1 O3 80.10(7) . . ?
F005 Sb1 O1 74.68(6) . 2_676 ?
O2 Sb1 O3 152.19(6) . . ?
O2 Sb1 O1 69.27(6) . 2_676 ?
O3 Sb1 O1 128.01(6) . 2_676 ?
F003 Sb2 O7 76.79(6) . . ?
F003 Sb2 O8 143.51(6) . 2_756 ?
F003 Sb2 O6 78.56(6) . . ?
F006 Sb2 F003 85.66(7) . . ?
F006 Sb2 O7 83.39(7) . . ?
F006 Sb2 O8 77.03(6) . 2_756 ?
F006 Sb2 O6 78.07(7) . . ?
O7 Sb2 O8 69.56(6) . 2_756 ?
O7 Sb2 O6 150.08(6) . . ?
O6 Sb2 O8 127.26(6) . 2_756 ?
C4 O7 Sb2 120.69(15) . . ?
C1 O2 Sb1 121.61(15) . . ?
C2 O3 Sb1 123.38(16) . . ?
H5A N5 H5B 120.0 . . ?
C6 N5 H5A 120.0 . . ?
C6 N5 H5B 120.0 . . ?
C4 O8 Sb2 113.37(15) . 2_756 ?
C3 O6 Sb2 122.94(17) . . ?
C1 O1 Sb1 112.88(15) . 2_676 ?
H9A O9 H9B 104.5 . . ?
H6A N6 H6B 120.0 . . ?
C6 N6 H6A 120.0 . . ?
C6 N6 H6B 120.0 . . ?
H2A N2 H2B 126(3) . . ?
C5 N2 H2A 114(2) . . ?
C5 N2 H2B 119(2) . . ?
H1A N1 H1B 120.0 . . ?
C5 N1 H1A 120.0 . . ?
C5 N1 H1B 120.0 . . ?
H8A N8 H8B 109.0 . . ?
N7 N8 H8A 109.3 . . ?
N7 N8 H8B 109.9 . . ?
N8 N7 H7 120.1 . . ?
C6 N7 N8 119.9(2) . . ?
C6 N7 H7 120.1 . . ?
H4A N4 H4B 102.2 . . ?
N3 N4 H4A 110.0 . . ?
N3 N4 H4B 105(3) . . ?
N4 N3 H3 120.4 . . ?
C5 N3 N4 119.1(2) . . ?
C5 N3 H3 120.4 . . ?
N6 C6 N5 120.3(2) . . ?
N7 C6 N5 119.9(2) . . ?
N7 C6 N6 119.8(2) . . ?
O2 C1 C1 116.8(3) . 2_676 ?
O1 C1 O2 125.2(2) . . ?
O1 C1 C1 118.0(3) . 2_676 ?
O7 C4 C4 116.8(3) . 2_756 ?
O8 C4 O7 125.2(2) . . ?
O8 C4 C4 118.0(3) . 2_756 ?
N2 C5 N1 119.7(3) . . ?
N3 C5 N2 120.6(3) . . ?
N3 C5 N1 119.8(3) . . ?
O6 C3 C3 117.8(3) . 2_767 ?
O5 C3 O6 125.0(2) . . ?
O5 C3 C3 117.2(3) . 2_767 ?
O3 C2 C2 117.4(3) . 2_665 ?
O4 C2 O3 125.1(2) . . ?
O4 C2 C2 117.5(3) . 2_665 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sb1 F004 1.9916(15) . ?
Sb1 F005 1.9199(14) . ?
Sb1 O2 2.2230(17) . ?
Sb1 O3 2.3667(18) . ?
Sb1 O1 2.5010(18) 2_676 ?
Sb2 F003 1.9959(15) . ?
Sb2 F006 1.9107(14) . ?
Sb2 O7 2.2435(17) . ?
Sb2 O8 2.4701(18) 2_756 ?
Sb2 O6 2.3464(19) . ?
O7 C4 1.269(3) . ?
O2 C1 1.274(3) . ?
O3 C2 1.265(3) . ?
N5 H5A 0.8800 . ?
N5 H5B 0.8800 . ?
N5 C6 1.330(3) . ?
O8 C4 1.242(3) . ?
O4 C2 1.244(3) . ?
O6 C3 1.260(3) . ?
O5 C3 1.247(3) . ?
O1 C1 1.235(3) . ?
O9 H9A 0.8704 . ?
O9 H9B 0.8696 . ?
N6 H6A 0.8800 . ?
N6 H6B 0.8800 . ?
N6 C6 1.329(3) . ?
N2 H2A 0.90(3) . ?
N2 C5 1.327(3) . ?
N2 H2B 0.87(3) . ?
N1 H1A 0.8800 . ?
N1 H1B 0.8800 . ?
N1 C5 1.329(4) . ?
N8 H8A 0.8834 . ?
N8 H8B 0.8833 . ?
N8 N7 1.411(3) . ?
N7 H7 0.8800 . ?
N7 C6 1.327(3) . ?
N4 H4A 0.8839 . ?
N4 N3 1.408(3) . ?
N4 H4B 0.79(4) . ?
N3 H3 0.8800 . ?
N3 C5 1.326(3) . ?
C1 C1 1.539(5) 2_676 ?
C4 C4 1.540(5) 2_756 ?
C3 C3 1.549(5) 2_767 ?
C2 C2 1.554(5) 2_665 ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Sb1 O2 C1 O1 170.13(18) . . . . ?
Sb1 O2 C1 C1 -10.4(3) . . . 2_676 ?
Sb1 O3 C2 O4 179.74(19) . . . . ?
Sb1 O3 C2 C2 -0.2(4) . . . 2_665 ?
Sb1 O1 C1 O2 171.59(19) 2_676 . . . ?
Sb1 O1 C1 C1 -7.9(3) 2_676 . . 2_676 ?
Sb2 O7 C4 O8 -169.77(18) . . . . ?
Sb2 O7 C4 C4 11.4(3) . . . 2_756 ?
Sb2 O8 C4 O7 -170.61(18) 2_756 . . . ?
Sb2 O8 C4 C4 8.2(3) 2_756 . . 2_756 ?
Sb2 O6 C3 O5 174.98(19) . . . . ?
Sb2 O6 C3 C3 -4.5(4) . . . 2_767 ?
N8 N7 C6 N5 179.7(2) . . . . ?
N8 N7 C6 N6 -1.0(4) . . . . ?
N4 N3 C5 N2 -2.8(4) . . . . ?
N4 N3 C5 N1 177.7(2) . . . . ?
