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_7708353
_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         'C43 H63 Co Mg N2 P2'
_chemical_formula_sum            'C43 H63 Co Mg N2 P2'
_chemical_formula_weight         753.13
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-07-27
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.16 svn.r6f6c53a7 for OlexSys, GUI svn.r6139)
;
_audit_update_record
;
2021-01-08 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            4
_cell_length_a                   16.8079(4)
_cell_length_b                   20.4351(4)
_cell_length_c                   11.6370(3)
_cell_measurement_reflns_used    11917
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      73.8070
_cell_measurement_theta_min      4.5740
_cell_volume                     3996.97(16)
_computing_cell_refinement       'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.14a (Rigaku OD, 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 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1773
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.982
_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   -117.00 -18.00   1.00    7.45    --  -42.10 -37.00 120.00   99
  2  \w     18.00 117.00   1.00    7.45    --   42.10  37.00  30.00   99
  3  \w      2.00  98.00   1.00    7.45    --   42.10-125.00 -90.00   96
  4  \w     30.00  69.00   1.00   29.78    --  106.40 -30.00  30.00   39
  5  \w     33.00 121.00   1.00   29.78    --  106.40-125.00 -90.00   88
  6  \w     33.00  77.00   1.00   29.78    --  106.40 -45.00  60.00   44
  7  \w     33.00 121.00   1.00   29.78    --  106.40-125.00-180.00   88
  8  \w     30.00  69.00   1.00   29.78    --  106.40 -30.00   0.00   39
  9  \w     30.00  69.00   1.00   29.78    --  106.40 -30.00-180.00   39
 10  \w     30.00  69.00   1.00   29.78    --  106.40 -30.00 150.00   39
 11  \w     30.00  69.00   1.00   29.78    --  106.40 -30.00 -60.00   39
 12  \w   -114.00 -60.00   1.00    7.45    --  -42.10-147.00-162.00   54
 13  \w   -114.00 -35.00   1.00    7.45    --  -42.10 -57.00  60.00   79
 14  \w   -114.00 -14.00   1.00    7.45    --  -42.10 -57.00-120.00  100
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Single source at offset/far, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0567456000
_diffrn_orient_matrix_UB_12      -0.0555146000
_diffrn_orient_matrix_UB_13      0.0361407000
_diffrn_orient_matrix_UB_21      0.0657787000
_diffrn_orient_matrix_UB_22      -0.0506316000
_diffrn_orient_matrix_UB_23      -0.0242675000
_diffrn_orient_matrix_UB_31      0.0292305000
_diffrn_orient_matrix_UB_32      0.0062702000
_diffrn_orient_matrix_UB_33      0.1250028000
_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  0.0355
_diffrn_reflns_av_unetI/netI     0.0228
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            20188
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.748
_diffrn_reflns_theta_min         4.327
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.506
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.444
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.14a (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'yellowish green'
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.252
_exptl_crystal_description       block
_exptl_crystal_F_000             1616
_exptl_crystal_size_max          0.493
_exptl_crystal_size_mid          0.311
_exptl_crystal_size_min          0.118
_refine_diff_density_max         1.389
_refine_diff_density_min         -0.551
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     239
_refine_ls_number_reflns         4086
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0577
_refine_ls_R_factor_gt           0.0558
_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^)+(0.0547P)^2^+7.6195P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1371
_refine_ls_wR_factor_ref         0.1384
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3936
_reflns_number_total             4086
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02621f2.cif
_cod_data_source_block           2m2m2m
_cod_database_code               7708353
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C H Co N P Mg'
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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:
 C20(H20)
2.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C12(H12A,H12B), C19(H19A,H19B), C22(H22A,H22B)
2.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C6(H6), C8(H8), C7(H7)
2.d Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C17(H17A,H17B,H17C), C3(H3A,H3B,
 H3C), C11(H11A,H11B,H11C), C13(H13A,H13B,H13C)
;
_shelx_res_checksum              94711
_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 2.438
_oxdiff_exptl_absorpt_empirical_full_min 0.615