Synthesis, crystallization and Hirshfeld surface analysis of transition metal carboxylate pentapyridines
Melvin, Marissa K.; Skelton, Brian W.; Eggers, Paul K.; Raston, Colin L.; CrystEngComm 24 (2022) 57–69; doi:10.1039/D1CE01248G

data_7243997
_publ_section_title
;
 Synthesis, crystallization and Hirshfeld surface analysis of transition
 metal carboxylate pentapyridines
;
_journal_issue                   1
_journal_name_full               CrystEngComm
_journal_page_first              57
_journal_page_last               69
_journal_paper_doi               10.1039/D1CE01248G
_journal_volume                  24
_journal_year                    2022
_chemical_absolute_configuration ad
_chemical_formula_moiety
'C30 H25 Co N5 O3, C F3 O3 S, C3 H6 O, 5(H2 O)'
_chemical_formula_sum            'C34 H41 Co F3 N5 O12 S'
_chemical_formula_weight         859.71
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      9
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   mixed
_audit_block_doi                 10.5517/ccdc.csd.cc1z8hqg
_audit_creation_date             2015-02-24T18:31:05-00:00
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_audit_update_record
;
2018-02-23 deposited with the CCDC.	2021-11-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.000(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.7330(5)
_cell_length_b                   12.1818(3)
_cell_length_c                   17.9613(5)
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_cell_measurement_temperature    100(2)
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_cell_measurement_theta_min      2.151
_cell_volume                     3660.64(17)
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;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
        (compiled Nov  6 2009,16:24:50)
;
_computing_data_collection
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        CrysAlisPro, Agilent Technologies,
        Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
        (compiled Nov  6 2009,16:24:50)
;
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        CrysAlisPro, Agilent Technologies,
        Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
        (compiled Nov  6 2009,16:24:50)
;
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_diffrn_ambient_temperature      100(2)
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_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.928
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0414776
_diffrn_orient_matrix_UB_12      -0.0111692
_diffrn_orient_matrix_UB_13      -0.0041167
_diffrn_orient_matrix_UB_21      0.0086297
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_diffrn_orient_matrix_UB_23      -0.0059449
_diffrn_orient_matrix_UB_31      -0.0023656
_diffrn_orient_matrix_UB_32      -0.0098084
_diffrn_orient_matrix_UB_33      0.038814
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
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_diffrn_reflns_av_unetI/netI     0.0532
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.928
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
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_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            19937
_diffrn_reflns_point_group_measured_fraction_full 0.922
_diffrn_reflns_point_group_measured_fraction_max 0.85
_diffrn_reflns_theta_full        31
_diffrn_reflns_theta_max         32.179
_diffrn_reflns_theta_min         2.268
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.612
_exptl_absorpt_correction_T_max  0.937
_exptl_absorpt_correction_T_min  0.826
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
     CrysAlisPro, Agilent Technologies,
Analytical numeric absorption correction using a multifaceted crystal
               model based on expressions derived by R.C. Clark & J.S.
        (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.56
_exptl_crystal_description       needle
_exptl_crystal_F_000             1784
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.637
_refine_diff_density_min         -0.342
_refine_diff_density_rms         0.075
_refine_ls_abs_structure_details
;
 Flack x determined using 3973 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.001(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     553
_refine_ls_number_reflns         10988
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0471
_refine_ls_R_factor_gt           0.0413
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0436P)^2^+0.5929P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0885
_refine_ls_wR_factor_ref         0.0927
_reflns_number_gt                10006
_reflns_number_total             10988
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01248g2.cif
_cod_data_source_block           cocooh
_cod_depositor_comments
'Adding full bibliography for 7243997--7243999.cif.'
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               7243997
_shelx_res_checksum              62864
_shelx_hkl_checksum              30018