Pyrazolate-supported Cr<sub>3</sub>(μ<sub>3</sub>-O) cores; homovalent CrIII3 and mixed-valent CrIII2Cr<sup>IV</sup>.
López-Plá, Jessica M; Obies, Mohammed; Zahariou, Georgia; Pissas, Michael; Sanakis, Yiannis; McGrady, John E.; Raptis, Raphael G.; Chemical communications (Cambridge, England) 60 (2024) 14117–14120; doi:10.1039/d4cc05161k

data_7133952
_publ_section_title
;
 Pyrazolate-supported Cr<sub>3</sub>(&#x3bc;<sub>3</sub>-O) cores;
 homovalent CrIII3 and mixed-valent CrIII2Cr<sup>IV</sup>.
;
_journal_issue                   95
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              14117
_journal_page_last               14120
_journal_paper_doi               10.1039/d4cc05161k
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C18 H12 Cl9 Cr3 N12 O, C H2 Cl2, 2(C24 H20 P)'
_chemical_formula_sum            'C67 H54 Cl11 Cr3 N12 O P2'
_chemical_formula_weight         1651.11
_chemical_name_common            '[PPh4]2[Cr3(m3-O)(m-4-Cl-pz)6Cl3],'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-03-24
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2024-05-27 deposited with the CCDC.	2024-11-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.746(5)
_cell_length_b                   17.540(4)
_cell_length_c                   16.981(4)
_cell_measurement_reflns_used    9937
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      24.250
_cell_measurement_theta_min      2.943
_cell_volume                     7073(3)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2016)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker D8 with PHOTON 100 detector'
_diffrn_measurement_method       '\f and \w shutterless scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1710
_diffrn_reflns_av_unetI/netI     0.1108
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            96314
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        24.803
_diffrn_reflns_theta_max         24.803
_diffrn_reflns_theta_min         2.888
_exptl_absorpt_coefficient_mu    0.967
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_correction_T_min  0.6863
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.551
_exptl_crystal_description       neddle
_exptl_crystal_F_000             3348
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH2Cl2, Et2O'
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.723
_refine_diff_density_min         -0.531
_refine_diff_density_rms         0.127
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.51(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     866
_refine_ls_number_reflns         12054
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.1208
_refine_ls_R_factor_gt           0.0713
_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^)+(0.0276P)^2^+57.8150P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1476
_refine_ls_wR_factor_ref         0.1667
_reflns_Friedel_coverage         0.924
_reflns_Friedel_fraction_full    0.989
_reflns_Friedel_fraction_max     0.989
_reflns_number_gt                8249
_reflns_number_total             12054
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc05161k2.cif
_cod_data_source_block           f_pl
_cod_depositor_comments
'Adding full bibliography for 7133952--7133953.cif.'
_cod_database_code               7133952
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.956
_shelx_estimated_absorpt_t_min   0.846
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.49(6)
 0.51(6)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
3.a Secondary CH2 refined with riding coordinates:
 C67(H67A,H67B)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C4(H4), C6(H6), C7(H7), C9(H9), C10(H10), C12(H12), C13(H13),
 C15(H15), C16(H16), C18(H18), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24),
  C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C32(H32), C33(H33),
 C34(H34), C35(H35), C36(H36), C38(H38), C39(H39), C40(H40), C41(H41), C42(H42),
  C44(H44), C45(H45), C46(H46), C47(H47), C48(H48), C50(H50), C51(H51),
 C52(H52), C53(H53), C54(H54), C56(H56), C57(H57), C58(H58), C59(H59), C60(H60),
  C62(H62), C63(H63), C64(H64), C65(H65), C66(H66)
;
_shelx_res_checksum              53241
_shelx_hkl_checksum              33783
_olex2_submission_special_instructions 'No special instructions were received'