#------------------------------------------------------------------------------
#$Date: 2022-05-12 10:41:53 +0300 (Thu, 12 May 2022) $
#$Revision: 275359 $
#$URL: file:///home/coder/svn-repositories/cod/cif/8/10/52/8105229.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_8105229
loop_
_publ_author_name
'Han, Min-Le'
'Li, Xiao-Dong'
'Li, Yan-Hong'
_publ_section_title
;
 Crystal structure of
 poly[diaqua-(μ3-3,4,5,6-tetrafluoro-phthalato-κ3O:O′:O′′)-(μ2-1,2-bis(4-pyridyl)ethene-κ2
 N:N′)cobalt(II)], C14H9CoF4NO6
;
_journal_issue                   3
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              593
_journal_page_last               594
_journal_paper_doi               10.1515/ncrs-2019-0837
_journal_volume                  235
_journal_year                    2020
_chemical_formula_moiety         'C14 H9 Co F4 N O6'
_chemical_formula_sum            'C14 H9 Co F4 N O6'
_chemical_formula_weight         422.15
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 90.672(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.1183(2)
_cell_length_b                   7.5688(2)
_cell_length_c                   32.5016(7)
_cell_measurement_reflns_used    3687
_cell_measurement_temperature    293
_cell_measurement_theta_max      73.4090
_cell_measurement_theta_min      5.4290
_cell_volume                     1504.99(7)
_computing_cell_refinement       'CrysAlisPro 1.171.39.9f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.9f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.9f (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
--------------------------------------------------------------------------
  1  ω    -45.00   3.00   0.50    0.50    --    0.00 -77.00  60.00   96
  2  ω    -31.00   9.00   0.50    0.50    --    0.00 -82.00  30.00   80
  3  ω    -12.00  14.00   0.50    0.50    --    0.00 -82.00 -90.00   52
  4  ω    -32.00   5.00   0.50    0.50    --    0.00 -82.00-180.00   74
  5  ω     67.00 120.00   0.50    1.97    --   95.20 -61.00   0.00  106
  6  ω     50.00 107.00   0.50    1.97    --   95.20 -77.00 120.00  114
  7  ω     17.00  61.00   0.50    1.97    --   95.20 -61.00   0.00   88
  8  ω     12.00  97.00   0.50    1.97    --   95.20 -45.00 150.00  170
  9  ω     99.00 183.00   0.50    1.97    --   95.20  45.00 -30.00  168
 10  ω     89.00 185.00   0.50    1.97    --   95.20  82.00  90.00  192
 11  ω     22.00 101.00   0.50    1.97    --   95.20 -30.00-180.00  158
 12  ω      6.00  35.00   0.50    1.97    --   95.20 -77.00 120.00   58
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Pro: Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0395578000
_diffrn_orient_matrix_UB_12      0.1767470000
_diffrn_orient_matrix_UB_13      0.0221958000
_diffrn_orient_matrix_UB_21      0.2349076000
_diffrn_orient_matrix_UB_22      -0.0051068000
_diffrn_orient_matrix_UB_23      0.0175629000
_diffrn_orient_matrix_UB_31      0.0814031000
_diffrn_orient_matrix_UB_32      0.1007918000
_diffrn_orient_matrix_UB_33      -0.0380466000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_av_unetI/netI     0.0474
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            7102
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        66.587
_diffrn_reflns_theta_max         66.587
_diffrn_reflns_theta_min         5.445
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.742
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.37414
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.9f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light pink'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.863
_exptl_crystal_description       block
_exptl_crystal_F_000             844
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0
_exptl_crystal_size_min          0
_refine_diff_density_max         0.430
_refine_diff_density_min         -0.389
_refine_diff_density_rms         0.072
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         2663
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0450
_refine_ls_R_factor_gt           0.0398
_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)+(0.0370P)²+1.6679P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1016
_refine_ls_wR_factor_ref         0.1037
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2385
_reflns_number_total             2663
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            suppl_ncrs-2019-0837_suppl.cif
_cod_data_source_block           10-23-4
_cod_database_code               8105229
_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   1.000
_shelx_estimated_absorpt_t_min   0.132
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 H6B-O6
 0.85 with sigma of 0.02
 H6A-O6
 0.85 with sigma of 0.02
3.a Rotating group:
 O5(H5A,H5B)
3.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C12(H12), C13(H13), C14(H14)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.489
_oxdiff_exptl_absorpt_empirical_full_min 0.668
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, 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
Co1 Co 0.37240(8) 0.35340(6) 0.29419(2) 0.02168(16) Uani 1 1 d . . . . .
F1 F -0.0368(4) 0.6877(3) 0.37152(6) 0.0443(5) Uani 1 1 d . . . . .
F2 F 0.1114(5) 0.7922(3) 0.44562(6) 0.0604(7) Uani 1 1 d . . . . .
F3 F 0.4991(5) 0.9662(3) 0.45256(6) 0.0643(8) Uani 1 1 d . . . . .
F4 F 0.7238(4) 1.0521(3) 0.38459(6) 0.0478(6) Uani 1 1 d . . . . .
O1 O 0.1779(4) 0.5852(3) 0.29129(7) 0.0302(5) Uani 1 1 d . . . . .
O2 O 0.1529(4) 0.8636(3) 0.27003(6) 0.0260(5) Uani 1 1 d . . . . .
O3 O 0.6625(4) 0.8567(3) 0.28218(8) 0.0370(6) Uani 1 1 d . . . . .
O4 O 0.5858(4) 1.1356(3) 0.29546(7) 0.0303(5) Uani 1 1 d . . . . .
O5 O 0.6614(4) 0.4968(3) 0.28730(6) 0.0284(5) Uani 1 1 d . . . . .
H5A H 0.6336 0.6085 0.2856 0.043 Uiso 1 1 d GR . . . .
H5B H 0.7197 0.4725 0.2639 0.043 Uiso 1 1 d GR . . . .
O6 O 0.0875(4) 0.1994(3) 0.29813(7) 0.0299(5) Uani 1 1 d D . . . .
N1 N 0.3860(4) 0.3744(3) 0.35996(7) 0.0250(6) Uani 1 1 d . . . . .
C1 C 0.1909(5) 0.7463(4) 0.29657(9) 0.0225(6) Uani 1 1 d . . . . .
C2 C 0.5782(5) 0.9746(4) 0.30318(9) 0.0245(7) Uani 1 1 d . . . . .
C3 C 0.2673(5) 0.8149(4) 0.33843(9) 0.0243(7) Uani 1 1 d . . . . .
C4 C 0.1536(5) 0.7761(4) 0.37358(9) 0.0292(7) Uani 1 1 d . . . . .
C5 C 0.2277(7) 0.8304(5) 0.41182(10) 0.0397(9) Uani 1 1 d . . . . .
C6 C 0.4223(7) 0.9201(5) 0.41535(10) 0.0391(9) Uani 1 1 d . . . . .
C7 C 0.5339(6) 0.9633(4) 0.38022(10) 0.0316(7) Uani 1 1 d . . . . .
C8 C 0.4576(5) 0.9164(4) 0.34157(9) 0.0229(6) Uani 1 1 d . . . . .
C9 C 0.5657(6) 0.4426(5) 0.37774(9) 0.0330(8) Uani 1 1 d . . . . .
H9 H 0.6824 0.4727 0.3611 0.040 Uiso 1 1 calc R . . . .
C10 C 0.5863(6) 0.4704(5) 0.41932(10) 0.0367(8) Uani 1 1 d . . . . .
H10 H 0.7134 0.5206 0.4301 0.044 Uiso 1 1 calc R . . . .
C11 C 0.4170(6) 0.4235(5) 0.44534(9) 0.0338(8) Uani 1 1 d . . . . .
C12 C 0.2330(6) 0.3503(5) 0.42707(10) 0.0362(8) Uani 1 1 d . . . . .
H12 H 0.1161 0.3155 0.4432 0.043 Uiso 1 1 calc R . . . .
C13 C 0.2225(6) 0.3286(5) 0.38472(10) 0.0321(8) Uani 1 1 d . . . . .
H13 H 0.0965 0.2802 0.3731 0.039 Uiso 1 1 calc R . . . .
C14 C 0.4261(7) 0.4523(5) 0.49001(10) 0.0415(9) Uani 1 1 d . . . . .
H14 H 0.3183 0.3987 0.5056 0.050 Uiso 1 1 calc R . . . .
H6A H 0.118(8) 0.096(3) 0.2886(13) 0.056(13) Uiso 1 1 d D . . . .
H6B H -0.035(5) 0.240(7) 0.2904(16) 0.088(19) Uiso 1 1 d D . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 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'
Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 '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'
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 Co1 N1 89.90(9) . .
O2 Co1 O1 83.70(8) 2_545 .
O2 Co1 O4 95.00(9) 2_545 1_545
O2 Co1 O6 91.69(9) 2_545 .
O2 Co1 N1 173.32(9) 2_545 .
O4 Co1 O1 175.53(9) 1_545 .
O4 Co1 N1 91.24(9) 1_545 .
O5 Co1 O1 92.34(9) . .
O5 Co1 O2 85.80(8) . 2_545
O5 Co1 O4 83.30(9) . 1_545
O5 Co1 O6 176.53(9) . .
O5 Co1 N1 92.60(9) . .
O6 Co1 O1 89.77(9) . .
O6 Co1 O4 94.55(9) . 1_545
O6 Co1 N1 90.17(10) . .
C1 O1 Co1 140.9(2) . .
C1 O2 Co1 131.98(19) . 2
C2 O4 Co1 138.3(2) . 1_565
Co1 O5 H5A 110.4 . .
Co1 O5 H5B 110.0 . .
H5A O5 H5B 103.7 . .
Co1 O6 H6A 107(3) . .
Co1 O6 H6B 121(4) . .
H6A O6 H6B 115(5) . .
C9 N1 Co1 118.7(2) . .
C13 N1 Co1 124.1(2) . .
C13 N1 C9 117.2(3) . .
O1 C1 O2 126.2(3) . .
O1 C1 C3 118.7(3) . .
O2 C1 C3 115.1(3) . .
O3 C2 O4 125.2(3) . .
O3 C2 C8 116.9(3) . .
O4 C2 C8 117.9(3) . .
C4 C3 C1 121.0(3) . .
C4 C3 C8 119.1(3) . .
C8 C3 C1 119.9(3) . .
F1 C4 C3 120.7(3) . .
F1 C4 C5 117.9(3) . .
C3 C4 C5 121.3(3) . .
F2 C5 C4 119.9(4) . .
F2 C5 C6 120.2(3) . .
C6 C5 C4 119.8(3) . .
F3 C6 C5 119.9(3) . .
F3 C6 C7 121.0(4) . .
C5 C6 C7 119.1(3) . .
F4 C7 C6 117.8(3) . .
F4 C7 C8 120.4(3) . .
C6 C7 C8 121.8(3) . .
C3 C8 C2 120.7(3) . .
C7 C8 C2 120.6(3) . .
C7 C8 C3 118.7(3) . .
N1 C9 H9 118.3 . .
N1 C9 C10 123.3(3) . .
C10 C9 H9 118.3 . .
C9 C10 H10 120.0 . .
C9 C10 C11 119.9(3) . .
C11 C10 H10 120.0 . .
C10 C11 C14 122.9(3) . .
C12 C11 C10 116.7(3) . .
C12 C11 C14 120.4(3) . .
C11 C12 H12 119.9 . .
C11 C12 C13 120.1(3) . .
C13 C12 H12 119.9 . .
N1 C13 C12 122.7(3) . .
N1 C13 H13 118.6 . .
C12 C13 H13 118.6 . .
C11 C14 H14 117.1 . .
C14 C14 C11 125.8(4) 3_666 .
C14 C14 H14 117.1 3_666 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 O1 2.121(2) .
Co1 O2 2.093(2) 2_545
Co1 O4 2.103(2) 1_545
Co1 O5 2.089(2) .
Co1 O6 2.102(2) .
Co1 N1 2.144(2) .
F1 C4 1.344(4) .
F2 C5 1.347(4) .
F3 C6 1.339(4) .
F4 C7 1.348(4) .
O1 C1 1.234(4) .
O2 Co1 2.093(2) 2
O2 C1 1.258(4) .
O3 C2 1.240(4) .
O4 Co1 2.103(2) 1_565
O4 C2 1.245(4) .
O5 H5A 0.8643 .
O5 H5B 0.8638 .
O6 H6A 0.863(19) .
O6 H6B 0.85(2) .
N1 C9 1.340(4) .
N1 C13 1.337(4) .
C1 C3 1.525(4) .
C2 C8 1.522(4) .
C3 C4 1.377(4) .
C3 C8 1.397(5) .
C4 C5 1.381(5) .
C5 C6 1.374(6) .
C6 C7 1.377(5) .
C7 C8 1.382(4) .
C9 H9 0.9300 .
C9 C10 1.372(4) .
C10 H10 0.9300 .
C10 C11 1.391(5) .
C11 C12 1.383(5) .
C11 C14 1.468(4) .
C12 H12 0.9300 .
C12 C13 1.387(5) .
C13 H13 0.9300 .
C14 C14 1.321(8) 3_666
C14 H14 0.9300 .
