Low-oxidation state cobalt‒magnesium complexes: ion-pairing and reactivity
Kelly, John A.; Gramüller, Johannes; Gschwind, Ruth M.; Wolf, Robert; Dalton Transactions  (2021) –; doi:10.1039/D1DT02621F

data_7708356
_publ_section_title
;
 Low-oxidation state cobalt--magnesium complexes: ion-pairing and
 reactivity
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT02621F
_journal_year                    2021
_chemical_formula_moiety         'C28 H45 Co Ni P2'
_chemical_formula_sum            'C28 H45 Co Ni P2'
_chemical_formula_weight         561.22
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-02-11
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6257)
;
_audit_update_record
;
2021-04-30 deposited with the CCDC.	2021-08-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.69710(10)
_cell_length_b                   13.92030(10)
_cell_length_c                   33.1444(2)
_cell_measurement_reflns_used    20096
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      75.1030
_cell_measurement_theta_min      2.6700
_cell_volume                     5396.81(7)
_computing_cell_refinement       'CrysAlisPro 1.171.41.81a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.81a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.81a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     61.00 108.00   0.50    0.78    --   79.50  21.00 117.27   94
  2  \w     69.00 114.00   0.50    0.78    --   79.50  20.00  49.67   90
  3  \w     61.00  87.00   0.50    0.78    --   79.50  17.00 -34.04   52
  4  \w     71.00  97.00   0.50    0.78    --   79.50  22.00   1.03   52
  5  \w     88.00 125.00   0.50    0.78    --   79.50  17.00 -34.04   74
  6  \w     93.00 123.00   0.50    0.78    --   79.50  20.00-140.23   60
  7  \w     58.00  89.00   0.50    0.78    --   79.50  20.00-140.23   62
  8  \w     59.00  99.00   0.50    0.78    --   79.50  16.00 -73.10   80
  9  \w     73.00 119.00   0.50    0.78    --   79.50   3.00  40.20   92
 10  \w     45.00 112.00   0.50    0.78    --   79.50   6.00 165.49  134
 11  \w     55.00  91.00   0.50    0.78    --   79.50  -1.00 -52.92   72
 12  \w     35.00  65.00   0.50    0.78    --   62.21 -95.00  30.00   60
 13  \w     38.00  63.00   0.50    0.78    --   75.56 -95.00 -60.00   50
 14  \w     36.00  61.00   0.50    0.78    --   79.50 -54.00  37.31   50
 15  \w     46.00  71.00   0.50    0.78    --   79.50-115.00-149.76   50
 16  \w     38.00  66.00   0.50    0.78    --   62.21 -95.00-150.00   56
 17  \w     24.00  49.00   0.50    0.78    --   62.21 -95.00-180.00   50
 18  \w   -103.00 -53.00   0.50    0.78    --  -70.22 -15.00-120.00  100
 19  \w   -115.00 -40.00   0.50    0.78    --  -70.22 -15.00 -30.00  150
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix-Arc 150'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1072607000
_diffrn_orient_matrix_UB_12      0.0406010000
_diffrn_orient_matrix_UB_13      0.0208931000
_diffrn_orient_matrix_UB_21      0.0075518000
_diffrn_orient_matrix_UB_22      -0.0797286000
_diffrn_orient_matrix_UB_23      0.0321210000
_diffrn_orient_matrix_UB_31      0.0760227000
_diffrn_orient_matrix_UB_32      0.0651837000
_diffrn_orient_matrix_UB_33      0.0262989000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0257
_diffrn_reflns_av_unetI/netI     0.0161
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            31428
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.135
_diffrn_reflns_theta_min         2.666
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.888
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66730
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.81a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.381
_exptl_crystal_description       block
_exptl_crystal_F_000             2384
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.331
_refine_diff_density_min         -0.221
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     300
_refine_ls_number_reflns         5511
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0260
_refine_ls_R_factor_gt           0.0246
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0359P)^2^+2.5626P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0663
_refine_ls_wR_factor_ref         0.0669
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5248
_reflns_number_total             5511
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02621f2.cif
_cod_data_source_block           jkc45
_cod_database_code               7708356
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C H P Co Ni'
_shelx_estimated_absorpt_t_max   0.546
_shelx_estimated_absorpt_t_min   0.340
_reflns_odcompleteness_completeness 99.25
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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:
 C11(H11), C15(H15), C12(H12), C16(H16)
2.b Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C18(H18A,H18B), C14(H14A,H14B), C17(H17A,H17B)
2.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C27(H27A,H27B,H27C), C9(H9A,H9B,H9C),
 C5(H5A,H5B,H5C), C26(H26A,H26B,H26C), C28(H28A,H28B,H28C), C4(H4A,H4B,H4C),
 C3(H3A,H3B,H3C), C25(H25A,H25B,H25C), C24(H24A,H24B,H24C)
;
_shelx_res_checksum              79751
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.678
_oxdiff_exptl_absorpt_empirical_full_min 0.553