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_7243998
_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_formula_moiety         'C60 H58 Cu4 N10 O10, 4(C F3 O3 S), 4(H2 O)'
_chemical_formula_sum            'C64 H66 Cu4 F12 N10 O26 S4'
_chemical_formula_weight         2001.67
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_doi                 10.5517/ccdc.csd.cc1z8j2v
_audit_creation_date             2014-05-13T10:00:38-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2018-02-23 deposited with the CCDC.	2021-11-24 downloaded from the CCDC.
;
_cell_angle_alpha                68.163(3)
_cell_angle_beta                 65.870(3)
_cell_angle_gamma                64.215(3)
_cell_formula_units_Z            1
_cell_length_a                   12.5531(4)
_cell_length_b                   13.0741(4)
_cell_length_c                   14.6993(5)
_cell_measurement_reflns_used    19791
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      67.234
_cell_measurement_theta_min      3.352
_cell_volume                     1926.33(12)
_computing_cell_refinement
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
        (compiled Nov  6 2009,16:24:50)
;
_computing_data_collection
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
        (compiled Nov  6 2009,16:24:50)
;
_computing_data_reduction
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
        (compiled Nov  6 2009,16:24:50)
;
_computing_molecular_graphics    'Diamond (Brandenburg, K., (1999)'
_computing_publication_material  'WinGX Farrugia, L. J. (1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2015)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4738
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction Gemini diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0253075
_diffrn_orient_matrix_UB_12      -0.1076575
_diffrn_orient_matrix_UB_13      0.0834856
_diffrn_orient_matrix_UB_21      -0.0162194
_diffrn_orient_matrix_UB_22      0.0552395
_diffrn_orient_matrix_UB_23      0.082935
_diffrn_orient_matrix_UB_31      -0.139464
_diffrn_orient_matrix_UB_32      0.059126
_diffrn_orient_matrix_UB_33      0.0109322
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0398
_diffrn_reflns_av_unetI/netI     0.024
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            38896
_diffrn_reflns_theta_full        67.39
_diffrn_reflns_theta_max         67.39
_diffrn_reflns_theta_min         3.39
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    3.279
_exptl_absorpt_correction_T_max  0.833
_exptl_absorpt_correction_T_min  0.531
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
     CrysAlisPro, Oxford Diffraction Ltd.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.725
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.647
_refine_diff_density_min         -0.32
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     579
_refine_ls_number_reflns         6854
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0448
_refine_ls_R_factor_gt           0.0374
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0644P)^2^+1.5314P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0989
_refine_ls_wR_factor_ref         0.1062
_reflns_number_gt                5933
_reflns_number_total             6854
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            d1ce01248g2.cif
_cod_data_source_block           cucooh
_cod_depositor_comments
'Adding full bibliography for 7243997--7243999.cif.'
_cod_original_cell_volume        1926.33(11)
_cod_original_sg_symbol_Hall     '-p 1'
_cod_database_code               7243998