Crystal structure of catena-poly[diaqua-bis(3,5-dichloropyridine-4-carboxylato-κ1 O)-bis(μ2-4,4′-bipyridine-κ2 N:N′)cobalt(II)], C22H16Cl4CoN4O6
Li, Xiao-Ling; Feng, Kai-Xin; Xin, Ling-Yun; Zeitschrift für Kristallographie - New Crystal Structures 234 (2019) 639–640; doi:10.1515/ncrs-2018-0592

data_8105805
_publ_section_title
;
 Crystal structure of
 catena-poly[diaqua-bis(3,5-dichloropyridine-4-carboxylato-\k1
 O)-bis(\m2-4,4&#x2032;-bipyridine-\k2 N:N&#x2032;)cobalt(II)],
 C22H16Cl4CoN4O6
;
_journal_issue                   4
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              639
_journal_page_last               640
_journal_paper_doi               10.1515/ncrs-2018-0592
_journal_volume                  234
_journal_year                    2019
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C11 H8 Cl2 Co0.5 N2 O3'
_chemical_formula_sum            'C11 H8 Cl2 Co0.5 N2 O3'
_chemical_formula_weight         316.56
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.1837(5)
_cell_length_b                   11.2878(6)
_cell_length_c                   11.3984(4)
_cell_measurement_reflns_used    3467
_cell_measurement_temperature    290.6(2)
_cell_measurement_theta_max      25.6420
_cell_measurement_theta_min      3.9910
_cell_volume                     1310.26(11)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41r (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_environment      air
_diffrn_ambient_temperature      290.6(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0584
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.980
_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    -51.00  59.00   1.00   10.00    --  -12.53  15.00  15.00  110
  2  \w    -82.00   6.00   1.00   10.00    --  -12.53 -38.00-180.00   88
  3  \w    -20.00  26.00   1.00   10.00    --  -12.53 -99.00   0.00   46
  4  \w    -20.00  26.00   1.00   10.00    --  -12.53 -99.00 120.00   46
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0566465000
_diffrn_orient_matrix_UB_12      0.0362952000
_diffrn_orient_matrix_UB_13      -0.0043357000
_diffrn_orient_matrix_UB_21      -0.0388203000
_diffrn_orient_matrix_UB_22      0.0507807000
_diffrn_orient_matrix_UB_23      0.0119003000
_diffrn_orient_matrix_UB_31      0.0116011000
_diffrn_orient_matrix_UB_32      -0.0073128000
_diffrn_orient_matrix_UB_33      0.0609230000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0337
_diffrn_reflns_av_unetI/netI     0.0432
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7778
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.498
_diffrn_reflns_theta_min         3.233
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.108
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83402
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41r (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.605
_exptl_crystal_description       block
_exptl_crystal_F_000             638
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.27
_refine_diff_density_max         0.401
_refine_diff_density_min         -0.261
_refine_diff_density_rms         0.057
_refine_ls_abs_structure_details
;
 Flack x determined using 788 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.487(11)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     176
_refine_ls_number_reflns         2393
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_gt           0.0400
_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^)+(0.0421P)^2^+0.7654P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0879
_refine_ls_wR_factor_ref         0.0910
_reflns_Friedel_coverage         0.713
_reflns_Friedel_fraction_full    0.984
_reflns_Friedel_fraction_max     0.976
_reflns_number_gt                2167
_reflns_number_total             2393
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2018-0592_suppl.cif
_cod_data_source_block           xly-19
_cod_original_formula_sum        'C11 H8 Cl2 Co0.50 N2 O3'
_cod_database_code               8105805
_reflns_odcompleteness_completeness 99.55
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.66
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Riding coordinates:
 O1W(H1WA,H1WB)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C5(H5), C6(H6), C10(H10), C11(H11)
;
_olex2_date_sample_data_collection 2017-05-08
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.286
_oxdiff_exptl_absorpt_empirical_full_min 0.735