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_7248883
_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
'C104 H84 Co5 N20 O16 P4, 7(C6 H6), 6(B F4), 4(C2 H3 N)'
_chemical_formula_sum            'C154 H138 B6 Co5 F24 N24 O16 P4'
_chemical_formula_weight         3520.27
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'I 2y'
_space_group_name_H-M_alt        'I 1 2 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2024-05-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2024-05-10 deposited with the CCDC.	2024-06-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.08(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   20.379(4)
_cell_length_b                   20.997(4)
_cell_length_c                   20.579(4)
_cell_measurement_reflns_used    2776
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.0
_cell_measurement_theta_min      0.4
_cell_volume                     8800(3)
_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)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.990
_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  0.0492
_diffrn_reflns_av_unetI/netI     0.0492
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            34571
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.102
_diffrn_reflns_theta_min         1.381
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.587
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_description       plate
_exptl_crystal_F_000             3598
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile/benzene'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.721
_refine_diff_density_min         -1.202
_refine_diff_density_rms         0.100
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.066(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1074
_refine_ls_number_reflns         19143
_refine_ls_number_restraints     186
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0652
_refine_ls_R_factor_gt           0.0613
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1169P)^2^+13.2822P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1604
_refine_ls_wR_factor_ref         0.1645
_reflns_Friedel_coverage         0.936
_reflns_Friedel_fraction_full    0.977
_reflns_Friedel_fraction_max     0.979
_reflns_number_gt                17926
_reflns_number_total             19143
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00468j2.cif
_cod_data_source_block           JSW-03-141-176-KY5_sq
_cod_depositor_comments
'Adding full bibliography for 7248881--7248883.cif.'
_cod_original_sg_symbol_H-M      I2
_cod_database_code               7248883
_shelxl_version_number           2014/6
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.934(15)
 0.066(15)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C743-C742 = C743-C741_$2 = C742-C741 = C743_$2-C741 = C743_$2-C742_$2 =
 C742_$2-C741_$2
 1.4 with sigma of 0.01
 C761-C762 = C763-C762 = C761_$1-C762_$1 = C763_$1-C762_$1
 1.4 with sigma of 0.01
 C761-C761_$1 = C763-C763_$1
 1.4 with sigma of 0.005
 C751-C752 = C753-C752 = C754-C753
 1.4 with sigma of 0.01
4. Restrained planarity
 C761_$1, C761, C762, C762_$1, C763_$1, C763
 with sigma of 0.05
5. Rigid bond restraints
 F522, F523, F524, F525, B521
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 F512, F513, F514, F515, B511
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
6. Uiso/Uaniso restraints and constraints
F522 \\sim F523 \\sim F524 \\sim F525 \\sim B521: within 1.7A with sigma of
0.02 and sigma for terminal atoms of 0.04
F512 \\sim F513 \\sim F514 \\sim F515 \\sim B511: within 1.7A with sigma of
0.02 and sigma for terminal atoms of 0.04
Uanis(C623) \\sim Ueq: with sigma of 0.025 and sigma for terminal atoms of 0.05
7. Rigid body (RIGU) restrains
 C741, C742, C743
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C761, C762, C763
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C751, C752, C753, C754
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 F522, F523, F524, F525, B521
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 F532, F533, F534, F535, B531
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
8. Others
 Fixed Sof: C751(0.25) H751(0.25) C752(0.5) H752(0.5) C753(0.5) H753(0.5)
 C754(0.25) H754(0.25) C761(0.5) H761(0.5) C762(0.5) H762(0.5) C763(0.5)
 H763(0.5)
 Fixed X: H62A(0.45982) H62B(0.454569) H62C(0.393121)
 Fixed Y: H62A(0.18503) H62B(0.2389) H62C(0.19693)
 Fixed Z: H62A(0.644629) H62B(0.69694) H62C(0.67827)
9.a Free rotating group:
 B531(F532,F533,F534,F535)
9.b Aromatic/amide H refined with riding coordinates:
 C112(H112), C114(H114), C115(H115), C116(H116), C118(H118), C120(H120),
 C121(H121), C122(H122), C123(H123), C212(H212), C214(H214), C215(H215),
 C216(H216), C218(H218), C220(H220), C221(H221), C222(H222), C223(H223),
 C312(H312), C314(H314), C315(H315), C316(H316), C318(H318), C320(H320),
 C321(H321), C322(H322), C323(H323), C412(H412), C414(H414), C415(H415),
 C416(H416), C418(H418), C420(H420), C421(H421), C422(H422), C423(H423),
 C711(H711), C712(H712), C713(H713), C714(H714), C715(H715), C716(H716),
 C721(H721), C722(H722), C723(H723), C724(H724), C725(H725), C726(H726),
 C731(H731), C732(H732), C733(H733), C734(H734), C751(H751), C752(H752),
 C753(H753), C754(H754), C741(H741), C742(H742), C743(H743), C761(H761),
 C762(H762), C763(H763)
9.c Idealised Me refined as rotating group:
 C53(H53A,H53B,H53C), C63(H63A,H63B,H63C), C613(H61A,H61B,H61C)
;
_shelx_res_checksum              27334
_shelx_hkl_checksum              25110
_shelx_fab_checksum              68969
_olex2_submission_special_instructions 'No special instructions were received'