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
Han, Min-Le; Li, Xiao-Dong; Li, Yan-Hong; Zeitschrift für Kristallographie - New Crystal Structures 235 (2020) 593–594; doi:10.1515/ncrs-2019-0837

data_8105229
_publ_section_title
;
 Crystal structure of
 poly[diaqua-(\m3-3,4,5,6-tetrafluoro-phthalato-\k3O:O&#x2032;:O&#x2032;&#x2032;)-(\m2-1,2-bis(4-pyridyl)ethene-\k2
 N:N&#x2032;)cobalt(II)], C14H9CoF4NO6
;
_journal_issue                   3
_journal_name_full
'Zeitschrift f\"ur 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  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -45.00   3.00   0.50    0.50    --    0.00 -77.00  60.00   96
  2  \w    -31.00   9.00   0.50    0.50    --    0.00 -82.00  30.00   80
  3  \w    -12.00  14.00   0.50    0.50    --    0.00 -82.00 -90.00   52
  4  \w    -32.00   5.00   0.50    0.50    --    0.00 -82.00-180.00   74
  5  \w     67.00 120.00   0.50    1.97    --   95.20 -61.00   0.00  106
  6  \w     50.00 107.00   0.50    1.97    --   95.20 -77.00 120.00  114
  7  \w     17.00  61.00   0.50    1.97    --   95.20 -61.00   0.00   88
  8  \w     12.00  97.00   0.50    1.97    --   95.20 -45.00 150.00  170
  9  \w     99.00 183.00   0.50    1.97    --   95.20  45.00 -30.00  168
 10  \w     89.00 185.00   0.50    1.97    --   95.20  82.00  90.00  192
 11  \w     22.00 101.00   0.50    1.97    --   95.20 -30.00-180.00  158
 12  \w      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       '\w 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/[\s^2^(Fo^2^)+(0.0370P)^2^+1.6679P] where P=(Fo^2^+2Fc^2^)/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 > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2019-0837_suppl.cif
_cod_data_source_block           10-23-4
_cod_database_code               8105229
_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