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_7708357
_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         'C41 H57 Co Mg N2'
_chemical_formula_sum            'C41 H57 Co Mg N2'
_chemical_formula_weight         661.12
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_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                 92.341(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.06340(10)
_cell_length_b                   13.9493(2)
_cell_length_c                   27.4651(5)
_cell_measurement_reflns_used    11311
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      73.6630
_cell_measurement_theta_min      4.5020
_cell_volume                     3469.46(9)
_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 0.991
_diffrn_measured_fraction_theta_max 0.961
_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 -15.00   1.00   16.34    --  -41.08 -37.00 -30.00  102
  2  \w    -20.00  83.00   1.00   16.34    --   41.08 -99.00-180.00  103
  3  \w     32.00  77.00   1.00   65.36    --  106.98 -45.00   0.00   45
  4  \w     29.00  69.00   1.00   65.36    --  106.98 -30.00 150.00   40
  5  \w     29.00  69.00   1.00   65.36    --  106.98 -30.00-180.00   40
  6  \w     23.00 109.00   1.00   65.36    --  106.98 -94.00 120.00   86
  7  \w     23.00 109.00   1.00   65.36    --  106.98 -94.00   0.00   86
  8  \w     73.00 158.00   1.00   65.36    --  106.98  77.00  90.00   85
  9  \w     73.00 158.00   1.00   65.36    --  106.98 125.00  30.00   85
 10  \w   -115.00 -11.00   1.00   16.34    --  -41.08 -57.00-180.00  104
 11  \w   -115.00 -11.00   1.00   16.34    --  -41.08 -57.00  90.00  104
 12  \w     46.00 158.00   1.00   65.36    --  106.98  15.00 -90.00  112
 13  \w     79.00 119.00   1.00   65.36    --  106.98  45.00 -30.00   40
;
_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      -0.0687576000
_diffrn_orient_matrix_UB_12      0.0744785000
_diffrn_orient_matrix_UB_13      -0.0356343000
_diffrn_orient_matrix_UB_21      0.1041259000
_diffrn_orient_matrix_UB_22      0.0774749000
_diffrn_orient_matrix_UB_23      0.0218353000
_diffrn_orient_matrix_UB_31      0.1154846000
_diffrn_orient_matrix_UB_32      -0.0255971000
_diffrn_orient_matrix_UB_33      -0.0375061000
_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  0.0211
_diffrn_reflns_av_unetI/netI     0.0217
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            20055
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.675
_diffrn_reflns_theta_min         3.221
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.275
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.610
_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 yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.266
_exptl_crystal_description       block
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.136
_exptl_crystal_size_min          0.105
_refine_diff_density_max         0.429
_refine_diff_density_min         -0.279
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     432
_refine_ls_number_reflns         6739
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0328
_refine_ls_R_factor_gt           0.0299
_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^)+(0.0393P)^2^+1.2012P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0760
_refine_ls_wR_factor_ref         0.0777
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6286
_reflns_number_total             6739
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02621f2.cif
_cod_data_source_block           p2m
_cod_database_code               7708357
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C160 H212 Co4 Mg4 N12 '
_shelx_estimated_absorpt_t_max   0.662
_shelx_estimated_absorpt_t_min   0.360
_reflns_odcompleteness_completeness 99.00
_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:
 C39(H39), C34(H34), C26(H26), C30(H30), C31(H31)
2.b Secondary CH2 refined with riding coordinates:
 C28(H28a,H28b), C41(H41a,H41b), C12(H12a,H12b), C29(H29a,H29b), C40(H40a,
 H40b), C36(H36a,H36b), C33(H33a,H33b), C32(H32a,H32b), C14(H14a,H14b),
 C22(H22a,H22b), C24(H24a,H24b)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C8(H8), C9(H9), C10(H10), C20(H20), C18(H18), C19(H19)
2.d Idealised Me refined as rotating group:
 C4(H4a,H4b,H4c), C5(H5a,H5b,H5c), C15(H15a,H15b,H15c), C13(H13a,H13b,H13c),
 C23(H23a,H23b,H23c), C25(H25a,H25b,H25c)
;
_shelx_res_checksum              79158
_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 1.423
_oxdiff_exptl_absorpt_empirical_full_min 0.726