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_7708355
_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         'C16 H24 Co, C46 H63 Mg N8'
_chemical_formula_sum            'C62 H87 Co Mg N8'
_chemical_formula_weight         1027.63
_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             2021-01-08
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2021-01-08 deposited with the CCDC.	2021-08-10 downloaded from the CCDC.
;
_cell_angle_alpha                103.677(3)
_cell_angle_beta                 104.369(3)
_cell_angle_gamma                94.547(3)
_cell_formula_units_Z            2
_cell_length_a                   10.8784(4)
_cell_length_b                   16.6782(6)
_cell_length_c                   16.6923(7)
_cell_measurement_reflns_used    21309
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      73.8310
_cell_measurement_theta_min      4.2360
_cell_volume                     2819.8(2)
_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      123.00(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 0.986
_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    -98.00  -2.00   1.00    4.58    --  -42.29 125.00 -60.00   96
  2  \w     14.00 114.00   1.00    4.58    --   42.29  57.00-120.00  100
  3  \w    -30.00  70.00   1.00    4.58    --   42.29 -57.00  90.00  100
  4  \w    -32.00  67.00   1.00    4.58    --   42.29 -37.00 -60.00   99
  5  \w     24.00 109.00   1.00   18.33    --  106.40 -94.00   0.00   85
  6  \w     33.00  77.00   1.00   18.33    --  106.40 -45.00  90.00   44
  7  \w     30.00  69.00   1.00   18.33    --  106.40 -30.00   0.00   39
  8  \w     33.00 121.00   1.00   18.33    --  106.40-125.00-120.00   88
  9  \w     30.00  69.00   1.00   18.33    --  106.40 -30.00  30.00   39
 10  \w     30.00  69.00   1.00   18.33    --  106.40 -30.00-180.00   39
 11  \w     24.00 109.00   1.00   18.33    --  106.40 -94.00  30.00   85
 12  \w     30.00 139.00   1.00   18.33    --  106.40 -77.00  60.00  109
 13  \w     30.00  69.00   1.00   18.33    --  106.40 -30.00 -30.00   39
 14  \w     33.00 121.00   1.00   18.33    --  106.40-125.00   0.00   88
 15  \w     77.00 158.00   1.00   18.33    --  106.40  61.00 -90.00   81
 16  \w     30.00 139.00   1.00   18.33    --  106.40 -77.00 -90.00  109
 17  \w     73.00 158.00   1.00   18.33    --  106.40 125.00-180.00   85
 18  \w     30.00  69.00   1.00   18.33    --  106.40 -30.00  90.00   39
 19  \w     54.00 158.00   1.00   18.33    --  106.40  15.00-120.00  104
 20  \w     25.00 158.00   1.00   18.33    --  106.40 -15.00-150.00  133
 21  \w     24.00 109.00   1.00   18.33    --  106.40 -94.00-120.00   85
 22  \w     33.00 121.00   1.00   18.33    --  106.40-125.00 150.00   88
 23  \w   -118.00 -10.00   1.00    4.58    --  -42.29 -77.00 120.00  108
 24  \w    -32.00  67.00   1.00    4.58    --   42.29 -37.00-180.00   99
 25  \w     14.00 114.00   1.00    4.58    --   42.29  57.00 -30.00  100
 26  \w     14.00 114.00   1.00    4.58    --   42.29  57.00  60.00  100
 27  \w     14.00 114.00   1.00    4.58    --   42.29  57.00 150.00  100
 28  \w     81.00 158.00   1.00   18.33    --  106.40  45.00 -30.00   77
 29  \w     78.00 158.00   1.00   18.33    --  106.40  30.00  30.00   80
 30  \w     81.00 158.00   1.00   18.33    --  106.40  45.00  90.00   77
;
_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      0.1149045000
_diffrn_orient_matrix_UB_12      0.0522260000
_diffrn_orient_matrix_UB_13      0.0729102000
_diffrn_orient_matrix_UB_21      -0.0605430000
_diffrn_orient_matrix_UB_22      -0.0247069000
_diffrn_orient_matrix_UB_23      0.0665315000
_diffrn_orient_matrix_UB_31      0.0705141000
_diffrn_orient_matrix_UB_32      -0.0767973000
_diffrn_orient_matrix_UB_33      -0.0046174000
_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  0.0259
_diffrn_reflns_av_unetI/netI     0.0204
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            42812
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.011
_diffrn_reflns_theta_min         3.390
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.839
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.361
_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 orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.210
_exptl_crystal_description       block
_exptl_crystal_F_000             1108
_exptl_crystal_size_max          0.428
_exptl_crystal_size_mid          0.294
_exptl_crystal_size_min          0.125
_refine_diff_density_max         0.446
_refine_diff_density_min         -0.279
_refine_diff_density_rms         0.038
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     661
_refine_ls_number_reflns         11287
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0340
_refine_ls_R_factor_gt           0.0324
_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^)+(0.0474P)^2^+0.8083P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0860
_refine_ls_wR_factor_ref         0.0873
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10846
_reflns_number_total             11287
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02621f2.cif
_cod_data_source_block           pbar
_cod_original_cell_volume        2819.80(19)
_cod_database_code               7708355
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C126 H174 Co2 Mg2 N14 '
_reflns_odcompleteness_completeness 99.96
_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:
 C48(H48), C45(H45), C52(H52), C44(H44), C53(H53), C49(H49), C57(H57), C56(H56)
2.b Secondary CH2 refined with riding coordinates:
 C14(H14a,H14b), C22(H22a,H22b), C12(H12a,H12b), C51(H51a,H51b), C50(H50a,
 H50b), C47(H47a,H47b), C46(H46a,H46b), C24(H24a,H24b), C58(H58a,H58b),
 C54(H54a,H54b), C55(H55a,H55b), C59(H59a,H59b)
2.c Aromatic/amide H refined with riding coordinates:
 C38(H38), C2(H2), C34(H34), C8(H8), C41(H41), C32(H32), C10(H10), C27(H27),
 C39(H39), C33(H33), C40(H40), C28(H28), C35(H35), C29(H29), C20(H20), C26(H26),
  C9(H9), C18(H18), C19(H19)
2.d Idealised Me refined as rotating group:
 C4(H4a,H4b,H4c), C13(H13a,H13b,H13c), C36(H36a,H36b,H36c), C5(H5a,H5b,H5c),
 C43(H43a,H43b,H43c), C15(H15a,H15b,H15c), C30(H30a,H30b,H30c), C23(H23a,H23b,
 H23c), C37(H37a,H37b,H37c), C31(H31a,H31b,H31c), C42(H42a,H42b,H42c), C25(H25a,
 H25b,H25c)
;
_shelx_res_checksum              80485
_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 1.592
_oxdiff_exptl_absorpt_empirical_full_min 0.746