A pentametallic Co5L4 architecture constructed from bis-substituted phosphate-based ligands
Ward, Jas S.; Kruger, Paul E.; CrystEngComm 26 (2024) 3459–3462; doi:10.1039/D4CE00468J

data_7248882
_publ_section_title
;
 A pentametallic Co5L4 architecture constructed from bis-substituted
 phosphate-based ligands
;
_journal_issue                   26
_journal_name_full               CrystEngComm
_journal_page_first              3459
_journal_page_last               3462
_journal_paper_doi               10.1039/D4CE00468J
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         'C24 H16 Co N6 O4, B F4, 2(C2 H3 N)'
_chemical_formula_sum            'C28 H22 B Co F4 N8 O4'
_chemical_formula_weight         680.27
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2016-08-30
_audit_creation_method
;
Olex2 1.2
(compiled 2016.08.25 svn.r3337 for OlexSys, GUI svn.r5221)
;
_audit_update_record
;
2017-08-18 deposited with the CCDC.	2024-06-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.62(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.803(3)
_cell_length_b                   16.333(3)
_cell_length_c                   14.884(3)
_cell_measurement_reflns_used    1167
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.0
_cell_measurement_theta_min      0.4
_cell_volume                     2873.0(12)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_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_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       '\f scans'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_source         'MX1 Beamline Australian Synchrotron'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0688
_diffrn_reflns_av_unetI/netI     0.0543
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            23903
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.282
_diffrn_reflns_theta_min         1.937
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.675
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.573
_exptl_crystal_description       plate
_exptl_crystal_F_000             1384
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: NCMe/benzene'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.699
_refine_diff_density_min         -1.151
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     417
_refine_ls_number_reflns         7032
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0787
_refine_ls_R_factor_gt           0.0550
_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^)+(0.0782P)^2^+2.4697P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1382
_refine_ls_wR_factor_ref         0.1538
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5225
_reflns_number_total             7032
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00468j2.cif
_cod_data_source_block           JSW-03-141-176-KY7
_cod_depositor_comments
'Adding full bibliography for 7248881--7248883.cif.'
_cod_original_cell_volume        2873.1(12)
_cod_database_code               7248882
_shelxl_version_number           2014/6
_exptl_absorpt_special_details   'XDS (Kabsch, 1993)'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C14(H14), C15(H15), C23(H23), C24(H24), C25(H25),
 C26(H26), C32(H32), C33(H33), C34(H34), C35(H35), C43(H43), C44(H44), C45(H45),
  C46(H46)
2.b Idealised Me refined as rotating group:
 C213(H21A,H21B,H21C), C223(H22A,H22B,H22C)
;
_shelx_res_checksum              59109
_shelx_hkl_checksum              9577
_olex2_submission_special_instructions 'No special instructions were received'