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_7708350
_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, C37 H57 Mg N2 O3, C4 H8 O'
_chemical_formula_sum            'C57 H87.47 Co Mg N2 O4'
_chemical_formula_weight         948.00
_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
_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                91.301(2)
_cell_angle_beta                 106.295(2)
_cell_angle_gamma                109.225(2)
_cell_formula_units_Z            2
_cell_length_a                   11.6935(3)
_cell_length_b                   14.9701(4)
_cell_length_c                   16.3882(4)
_cell_measurement_reflns_used    25244
_cell_measurement_temperature    122.94(15)
_cell_measurement_theta_max      73.6740
_cell_measurement_theta_min      4.1540
_cell_volume                     2578.95(12)
_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      122.94(15)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 4.2047
_diffrn_detector_type            TitanS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.976
_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   -114.00 -19.00   1.00    8.00    --  -44.65 -57.00 150.00   95
  2  \w   -118.00 -73.00   1.00    8.00    --  -44.65-125.00-150.00   45
  3  \w   -114.00 -19.00   1.00    8.00    --  -44.65 -57.00-120.00   95
  4  \w      1.00  84.00   1.00    8.00    --   44.65 -99.00  30.00   83
  5  \w     31.00  91.00   1.00   23.00    --  104.50 -30.00-180.00   60
  6  \w     30.00 136.00   1.00   23.00    --  104.50 -77.00  60.00  106
  7  \w     34.00  98.00   1.00   23.00    --  104.50 -45.00-120.00   64
  8  \w     80.00 175.00   1.00   23.00    --  104.50  45.00-150.00   95
  9  \w     31.00 118.00   1.00   23.00    --  104.50-125.00  60.00   87
 10  \w     21.00 110.00   1.00   23.00    --  104.50 -94.00-120.00   89
 11  \w     31.00 118.00   1.00   23.00    --  104.50-125.00-150.00   87
 12  \w     65.00 178.00   1.00   23.00    --  104.50  15.00 150.00  113
 13  \w   -118.00 -73.00   1.00    8.00    --  -44.65-125.00  90.00   45
 14  \w   -126.00 -79.00   1.00    8.00    --  -44.65 -99.00   0.00   47
 15  \w   -114.00 -19.00   1.00    8.00    --  -44.65 -57.00   0.00   95
 16  \w     80.00 175.00   1.00   23.00    --  104.50  45.00  60.00   95
 17  \w     80.00 175.00   1.00   23.00    --  104.50  45.00 -90.00   95
 18  \w     73.00 178.00   1.00   23.00    --  104.50  77.00 150.00  105
 19  \w     73.00 178.00   1.00   23.00    --  104.50  76.00-133.00  105
 20  \w     78.00 174.00   1.00   23.00    --  104.50  61.00   0.00   96
 21  \w     65.00 178.00   1.00   23.00    --  104.50  15.00   0.00  113
 22  \w   -119.00 -13.00   1.00    8.00    --  -44.65 -77.00 -30.00  106
 23  \w   -114.00 -19.00   1.00    8.00    --  -44.65 -57.00  90.00   95
 24  \w     23.00  98.00   1.00    8.00    --   44.65-125.00 -90.00   75
 25  \w     73.00 178.00   1.00   23.00    --  104.50  77.00 -90.00  105
 26  \w     78.00 174.00   1.00   23.00    --  104.50  61.00 -30.00   96
 27  \w     73.00 178.00   1.00   23.00    --  104.50  77.00  90.00  105
 28  \w     73.00 178.00   1.00   23.00    --  104.50  77.00   0.00  105
 29  \w     73.00 178.00   1.00   23.00    --  104.50  77.00  60.00  105
 30  \w     73.00 178.00   1.00   23.00    --  104.50  77.00 120.00  105
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'GV1000, TitanS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1086509000
_diffrn_orient_matrix_UB_12      0.0016024000
_diffrn_orient_matrix_UB_13      -0.0784769000
_diffrn_orient_matrix_UB_21      0.0363406000
_diffrn_orient_matrix_UB_22      0.1079119000
_diffrn_orient_matrix_UB_23      0.0243947000
_diffrn_orient_matrix_UB_31      0.0913283000
_diffrn_orient_matrix_UB_32      0.0206252000
_diffrn_orient_matrix_UB_33      -0.0547313000
_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  0.0413
_diffrn_reflns_av_unetI/netI     0.0250
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            48564
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.001
_diffrn_reflns_theta_min         3.152
_diffrn_source                   'gradient vaccum rotating-anode X-ray tube'
_diffrn_source_type              'GV1000 (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.083
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.333
_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 orangish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.221
_exptl_crystal_description       block
_exptl_crystal_F_000             1029
_exptl_crystal_size_max          0.716
_exptl_crystal_size_mid          0.282
_exptl_crystal_size_min          0.158
_refine_diff_density_max         0.428
_refine_diff_density_min         -0.458
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     603
_refine_ls_number_reflns         10227
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0471
_refine_ls_R_factor_gt           0.0451
_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^)+(0.0607P)^2^+1.5287P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1169
_refine_ls_wR_factor_ref         0.1188
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9753
_reflns_number_total             10227
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02621f2.cif
_cod_data_source_block           mgcothf
_cod_database_code               7708350
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C H N O Mg Co'
_reflns_odcompleteness_completeness 99.82
_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, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(H12C)=Sof(H12D)=Sof(C13B)=Sof(H13D)=Sof(H13E)=Sof(H13F)=1-FVAR(1)
 Sof(H12A)=Sof(H12B)=Sof(C13A)=Sof(H13A)=Sof(H13B)=Sof(H13C)=FVAR(1)
3.a Ternary CH refined with riding coordinates:
 C43(H43), C47(H47), C42(H42), C57(H57), C46(H46), C54(H54), C53(H53), C50(H50)
3.b Secondary CH2 refined with riding coordinates:
 C26(H26A,H26B), C22(H22A,H22B), C14(H14A,H14B), C33(H33A,H33B), C34(H34A,
 H34B), C37(H37A,H37B), C12(H12C,H12D), C12(H12A,H12B), C36(H36A,H36B),
 C35(H35A,H35B), C29(H29A,H29B), C56(H56A,H56B), C24(H24A,H24B), C27(H27A,H27B),
  C30(H30A,H30B), C40(H40A,H40B), C55(H55A,H55B), C28(H28A,H28B), C45(H45A,
 H45B), C39(H39A,H39B), C44(H44A,H44B), C32(H32A,H32B), C41(H41A,H41B),
 C38(H38A,H38B), C49(H49A,H49B), C31(H31A,H31B), C48(H48A,H48B), C52(H52A,H52B),
  C51(H51A,H51B)
3.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C10(H10), C18(H18), C20(H20), C9(H9), C8(H8), C19(H19)
3.d Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C4(H4A,H4B,H4C), C23(H23A,H23B,H23C), C15(H15A,H15B,H15C),
 C25(H25A,H25B,H25C), C13A(H13A,H13B,H13C), C13B(H13D,H13E,H13F)
;
_shelx_res_checksum              12176
_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 1.882
_oxdiff_exptl_absorpt_empirical_full_min 0.733