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_7243999
_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         'C30 H26 N5 Ni O3, C F3 O3 S, 2.27(H2 O)'
_chemical_formula_sum            'C31 H30.54 F3 N5 Ni O8.27 S'
_chemical_formula_weight         753.23
_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.cc1z8j3w
_audit_creation_date             2014-05-15T08:25:22-00:00
_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                104.917(2)
_cell_angle_beta                 98.643(2)
_cell_angle_gamma                113.012(3)
_cell_formula_units_Z            2
_cell_length_a                   11.0416(3)
_cell_length_b                   11.7979(4)
_cell_length_c                   14.2305(3)
_cell_measurement_reflns_used    16651
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      37.35
_cell_measurement_theta_min      3.703
_cell_volume                     1581.79(9)
_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, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4738
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction Gemini diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0543896
_diffrn_orient_matrix_UB_12      -0.0131717
_diffrn_orient_matrix_UB_13      0.0189036
_diffrn_orient_matrix_UB_21      0.0455229
_diffrn_orient_matrix_UB_22      0.0680944
_diffrn_orient_matrix_UB_23      0.0183092
_diffrn_orient_matrix_UB_31      -0.0161732
_diffrn_orient_matrix_UB_32      0.0064731
_diffrn_orient_matrix_UB_33      0.0468848
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0406
_diffrn_reflns_av_unetI/netI     0.0459
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            52816
_diffrn_reflns_theta_full        37
_diffrn_reflns_theta_max         37.68
_diffrn_reflns_theta_min         3.48
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.758
_exptl_absorpt_correction_T_max  0.927
_exptl_absorpt_correction_T_min  0.831
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
       CrysAlisPro, Oxford Diffraction Ltd.

;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.581
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             777
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.04
_refine_diff_density_min         -0.561
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.03
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     549
_refine_ls_number_reflns         16092
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0706
_refine_ls_R_factor_gt           0.0475
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0518P)^2^+0.5428P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1103
_refine_ls_wR_factor_ref         0.1221
_reflns_number_gt                12113
_reflns_number_total             16092
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            d1ce01248g2.cif
_cod_data_source_block           nicooh
_cod_depositor_comments
'Adding full bibliography for 7243997--7243999.cif.'
_cod_original_cell_volume        1581.79(8)
_cod_database_code               7243999