Crystal structure of (2-carboxy-4-(3-carboxy-5-carboxylatophenoxy)benzoato-κ2 O,O′)bis(1,10-phenantroline-κ2 N,N′)cobalt(II), C40H24N4O9Co
Luo, Jie; Gu, Guang-Na; Wang, Xiao-Wei; Zeitschrift für Kristallographie - New Crystal Structures 235 (2020) 1543–1545; doi:10.1515/ncrs-2020-0383

data_8105516
_publ_section_title
;
 Crystal structure of
 (2-carboxy-4-(3-carboxy-5-carboxylatophenoxy)benzoato-\k2
 O,O&#x2032;)bis(1,10-phenantroline-\k2 N,N&#x2032;)cobalt(II),
 C40H24N4O9Co
;
_journal_issue                   6
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              1543
_journal_page_last               1545
_journal_paper_doi               10.1515/ncrs-2020-0383
_journal_volume                  235
_journal_year                    2020
_chemical_formula_moiety         'C40 H24 Co N4 O9'
_chemical_formula_sum            'C40 H24 Co N4 O9'
_chemical_formula_weight         763.56
_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   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                82.003(8)
_cell_angle_beta                 77.597(7)
_cell_angle_gamma                76.048(8)
_cell_formula_units_Z            2
_cell_length_a                   11.5623(9)
_cell_length_b                   11.5732(12)
_cell_length_c                   13.4379(11)
_cell_measurement_reflns_used    10235
_cell_measurement_temperature    286.40(10)
_cell_measurement_theta_max      26.2010
_cell_measurement_theta_min      3.7350
_cell_volume                     1697.1(3)
_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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      286.40(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0584
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_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    -26.00  58.00   1.00    8.70    --   -9.62  57.00-180.00   84
  2  \w     -6.00  78.00   1.00    8.70    --   10.64  57.00 -30.00   84
  3  \w     -6.00  78.00   1.00    8.70    --   10.64  57.00 150.00   84
  4  \w    -20.00  50.00   1.00    8.70    --   10.64 -99.00 150.00   70
  5  \w     -6.00  78.00   1.00    8.70    --   10.64  57.00-120.00   84
  6  \w    -20.00  50.00   1.00    8.70    --   10.64 -99.00 -30.00   70
  7  \w    -20.00  50.00   1.00    8.70    --   10.64 -99.00-120.00   70
  8  \w    -20.00  50.00   1.00    8.70    --   10.64 -99.00  60.00   70
  9  \w     -8.00  80.00   1.00    8.70    --   10.64  38.00  90.00   88
 10  \w    -20.00  50.00   1.00    8.70    --   10.64 -99.00 -60.00   70
 11  \w    -20.00  39.00   1.00    8.70    --   10.64 -99.00-150.00   59
 12  \w    -57.00  37.00   1.00    8.70    --   10.64 -77.00  60.00   94
;
_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      -0.0411761000
_diffrn_orient_matrix_UB_12      0.0048346000
_diffrn_orient_matrix_UB_13      -0.0333935000
_diffrn_orient_matrix_UB_21      -0.0048863000
_diffrn_orient_matrix_UB_22      -0.0599840000
_diffrn_orient_matrix_UB_23      0.0158590000
_diffrn_orient_matrix_UB_31      -0.0492298000
_diffrn_orient_matrix_UB_32      0.0200195000
_diffrn_orient_matrix_UB_33      0.0397397000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0925
_diffrn_reflns_av_unetI/netI     0.0683
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            31165
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         3.31
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.572
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60676
_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            red
_exptl_crystal_density_diffrn    1.494
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             782
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.384
_refine_diff_density_min         -0.313
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     489
_refine_ls_number_reflns         6024
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0665
_refine_ls_R_factor_gt           0.0462
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0389P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0940
_refine_ls_wR_factor_ref         0.1021
_reflns_number_gt                4766
_reflns_number_total             6024
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            suppl_ncrs-2020-0383_suppl.cif
_cod_data_source_block           124
_cod_database_code               8105516
_chemical_oxdiff_formula         'c h n o co'
_reflns_odcompleteness_completeness 99.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     23.21
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C6(H6), C7(H7A), C10(H10), C11(H11), C12(H12),
 C13(H13), C14(H14), C15(H15), C18(H18), C19(H19), C22(H22), C23(H23), C24(H24),
  C27(H27), C29(H29), C31(H31), C34(H34), C37(H37), C38(H38)
2.b Idealised tetrahedral OH refined as rotating group:
 O5(H5), O7(H7)
;
_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 2.653
_oxdiff_exptl_absorpt_empirical_full_min 0.399