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_7708351
_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         'C45 H65 Co Mg N2'
_chemical_formula_sum            'C45 H65 Co Mg N2'
_chemical_formula_weight         717.23
_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   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            8
_cell_length_a                   19.3913(4)
_cell_length_b                   16.0799(4)
_cell_length_c                   24.4772(6)
_cell_measurement_reflns_used    7434
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      73.8830
_cell_measurement_theta_min      3.9760
_cell_volume                     7632.2(3)
_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  (Sheldrick, 2015)'
_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 0.999
_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    -65.00  30.00   1.00   25.00    --  -42.68  37.00-150.00   95
  2  \w   -117.00 -11.00   1.00   25.00    --  -42.68 -77.00-120.00  106
  3  \w     25.00  76.00   1.00   50.00    --  106.63 -94.00  90.00   51
  4  \w     34.00  67.00   1.00   50.00    --  106.63 -30.00 -30.00   33
  5  \w     33.00  69.00   1.00   50.00    --  106.63 -30.00 -60.00   36
  6  \w     34.00  61.00   1.00   50.00    --  106.63 -30.00   0.00   27
  7  \w     34.00  69.00   1.00   50.00    --  106.63 -30.00 -90.00   35
  8  \w     55.00 104.00   1.00   50.00    --  106.63 -94.00-180.00   49
  9  \w     48.00 130.00   1.00   50.00    --  106.63 -61.00-150.00   82
 10  \w     46.00  76.00   1.00   50.00    --  106.63 -45.00  60.00   30
;
_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      0.0686585000
_diffrn_orient_matrix_UB_12      -0.0142092000
_diffrn_orient_matrix_UB_13      -0.0303313000
_diffrn_orient_matrix_UB_21      -0.0397739000
_diffrn_orient_matrix_UB_22      -0.0147566000
_diffrn_orient_matrix_UB_23      -0.0535502000
_diffrn_orient_matrix_UB_31      0.0041792000
_diffrn_orient_matrix_UB_32      0.0935939000
_diffrn_orient_matrix_UB_33      -0.0131347000
_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  0.0419
_diffrn_reflns_av_unetI/netI     0.0414
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            23793
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.003
_diffrn_reflns_theta_min         3.612
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.925
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.425
_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            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.248
_exptl_crystal_description       plate
_exptl_crystal_F_000             3104
_exptl_crystal_size_max          0.357
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.044
_refine_diff_density_max         0.890
_refine_diff_density_min         -0.372
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     468
_refine_ls_number_reflns         7609
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_gt           0.0434
_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^)+(0.0508P)^2^+4.5225P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1009
_refine_ls_wR_factor_ref         0.1090
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6207
_reflns_number_total             7609
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02621f2.cif
_cod_data_source_block           pbca
_cod_database_code               7708351
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C336 H496 Co8 Mg8 N40 '
_shelx_estimated_absorpt_t_max   0.846
_shelx_estimated_absorpt_t_min   0.335
_reflns_odcompleteness_completeness 99.85
_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:
 C32(H32), C43(H43), C39(H39), C42(H42), C36(H36), C33(H33), C28(H28),
 C24(H24), C12(H12), C15(H15)
2.b Secondary CH2 refined with riding coordinates:
 C44(H44A,H44B), C34(H34A,H34B), C31(H31A,H31B), C40(H40A,H40B), C45(H45A,
 H45B), C35(H35A,H35B), C41(H41A,H41B)
2.c Aromatic/amide H refined with riding coordinates:
 C20(H20), C3(H3), C10(H10), C21(H21), C22(H22), C9(H9), C8(H8)
2.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C5(H5A,H5B,H5C), C29(H29A,H29B,H29C), C13(H13A,H13B,H13C),
 C27(H27A,H27B,H27C), C26(H26A,H26B,H26C), C14(H14A,H14B,H14C), C25(H25A,H25B,
 H25C), C17(H17A,H17B,H17C), C16(H16A,H16B,H16C)
;
_shelx_res_checksum              54792
_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 1.465
_oxdiff_exptl_absorpt_empirical_full_min 0.865