Phosphinoquinoline supported CoII, NiII, and FeII complexes: divergent behaviour upon reduction
SCHILTZ, pauline; Casaretto, Nicolas; Bourcier, Sophie; Gosmini, Corinne; Auffrant, Audrey; Dalton Transactions  (2023) –; doi:10.1039/D3DT02441E

data_7713986
_publ_section_title
;
 Phosphinoquinoline supported CoII, NiII, and FeII complexes: divergent
 behaviour upon reduction
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02441E
_journal_year                    2023
_chemical_absolute_configuration reference
_chemical_formula_moiety         'C45 H60 N3 Ni3 P3, [+ solvents]'
_chemical_formula_sum            'C45 H60 N3 Ni3 P3'
_chemical_formula_weight         912.00
_space_group_crystal_system      hexagonal
_space_group_IT_number           173
_space_group_name_Hall           'P 6c'
_space_group_name_H-M_alt        'P 63'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-04-28
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2023-07-26 deposited with the CCDC.	2023-09-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   15.101(2)
_cell_length_b                   15.101(2)
_cell_length_c                   12.0727(17)
_cell_measurement_reflns_used    1511
_cell_measurement_temperature    149.99
_cell_measurement_theta_max      19.73
_cell_measurement_theta_min      2.30
_cell_volume                     2384.2(6)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      149.99
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1513
_diffrn_reflns_av_unetI/netI     0.1314
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            24516
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.680
_diffrn_reflns_theta_min         1.557
_diffrn_source_current           31.0
_diffrn_source_power             1.705
_diffrn_source_voltage           55.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.305
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6960
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0977 before and 0.0825 after correction.
The Ratio of minimum to maximum transmission is 0.9332.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'dark brown'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.270
_exptl_crystal_description       block
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.500
_refine_diff_density_min         -0.528
_refine_diff_density_rms         0.136
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.00(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.901
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     168
_refine_ls_number_reflns         2997
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.900
_refine_ls_R_factor_all          0.0726
_refine_ls_R_factor_gt           0.0489
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0586P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0995
_refine_ls_wR_factor_ref         0.1280
_reflns_Friedel_coverage         0.878
_reflns_Friedel_fraction_full    0.973
_reflns_Friedel_fraction_max     0.972
_reflns_number_gt                2006
_reflns_number_total             2997
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02441e2.cif
_cod_data_source_block           psc676_0m
_cod_original_cell_volume        2384.3(7)
_cod_database_code               7713986
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.903
_shelx_estimated_absorpt_t_min   0.859
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 1.00(5)
 -0.00(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Ternary CH refined with riding coordinates:
 C2(H008), C3(H009), C00E(H00E), C00H(H00L)
3.b Aromatic/amide H refined with riding coordinates:
 C004(H004), C005(H005), C007(H007), C00A(H00A)
3.c Idealised Me refined as rotating group:
 C00B(H00B,H00C,H00D), C00F(H00F,H00G,H00H), C00G(H00I,H00J,H00K), C00I(H00M,
 H00N,H00O)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              36832
_shelx_fab_checksum              47546
_olex2_submission_special_instructions 'No special instructions were received'