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_7713981
_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_formula_moiety         'C30 H38 Br Co N2 P2, Br3 Co, C H2 Cl2'
_chemical_formula_sum            'C31 H40 Br4 Cl2 Co2 N2 P2'
_chemical_formula_weight         1010.99
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-07-09
_audit_creation_method
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_audit_update_record
;
2023-07-26 deposited with the CCDC.	2023-09-18 downloaded from the CCDC.
;
_cell_angle_alpha                109.871(4)
_cell_angle_beta                 100.733(4)
_cell_angle_gamma                109.062(4)
_cell_formula_units_Z            2
_cell_length_a                   11.6902(18)
_cell_length_b                   13.315(2)
_cell_length_c                   14.484(2)
_cell_measurement_reflns_used    5211
_cell_measurement_temperature    150.01
_cell_measurement_theta_max      23.401
_cell_measurement_theta_min      2.494
_cell_volume                     1888.6(5)
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150.01
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0874
_diffrn_reflns_av_unetI/netI     0.0878
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            33540
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.677
_diffrn_reflns_theta_min         1.586
_diffrn_source_current           31.0
_diffrn_source_power             1.705
_diffrn_source_voltage           55.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.360
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5876
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0990 before and 0.0677 after correction.
The Ratio of minimum to maximum transmission is 0.7881.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.778
_exptl_crystal_description       plate
_exptl_crystal_F_000             996
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.517
_refine_diff_density_min         -1.955
_refine_diff_density_rms         0.161
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     396
_refine_ls_number_reflns         7180
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.1021
_refine_ls_R_factor_gt           0.0580
_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^)+(0.0655P)^2^+10.2882P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1408
_refine_ls_wR_factor_ref         0.1644
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4773
_reflns_number_total             7180
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02441e2.cif
_cod_data_source_block           psc101_0m
_cod_database_code               7713981
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.900
_shelx_estimated_absorpt_t_min   0.414
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C00X(H00X), C00M(H00M), C010(H010), C011(H011)
2.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B)
2.c Aromatic/amide H refined with riding coordinates:
 C00Y(H00Y), C00P(H00P), C00Q(H00Q), C00T(H00T), C00V(H00V), C00U(H00U),
 C00O(H00O), C00N(H00N), C00H(H00J), C00I(H00K)
2.d Idealised Me refined as rotating group:
 C00Z(H00A,H00B,H00C), C00S(H00D,H00E,H00F), C00W(H00G,H00H,H00I), C012(H01A,
 H01B,H01C), C013(H01D,H01E,H01F), C014(H01G,H01H,H01I), C015(H01J,H01K,H01L),
 C016(H01M,H01N,H01O)
;
_shelx_res_checksum              50295
_olex2_submission_special_instructions 'No special instructions were received'