Magnesium-stabilised transition metal formyl complexes: structures, bonding, and ethenediolate formation.
Parr, Joseph M.; White, Andrew J. P.; Crimmin, Mark R.; Chemical science 13 (2022) 6592–6598; doi:10.1039/d2sc02063g

data_1566980
_publ_section_title
;
 Magnesium-stabilised transition metal formyl complexes: structures,
 bonding, and ethenediolate formation.
;
_journal_issue                   22
_journal_name_full               'Chemical science'
_journal_page_first              6592
_journal_page_last               6598
_journal_paper_doi               10.1039/d2sc02063g
_journal_volume                  13
_journal_year                    2022
_chemical_formula_moiety         'C67 H91 Mg2 Mn N4 O3'
_chemical_formula_sum            'C67 H91 Mg2 Mn N4 O3'
_chemical_formula_weight         1103.99
_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             2021-10-15
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2021-10-15 deposited with the CCDC.	2022-05-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.903(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.2588(7)
_cell_length_b                   12.9668(5)
_cell_length_c                   35.832(3)
_cell_measurement_reflns_used    5535
_cell_measurement_temperature    172.95(10)
_cell_measurement_theta_max      26.0450
_cell_measurement_theta_min      2.7560
_cell_volume                     7022.3(7)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      172.95(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0382
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.797
_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    -23.00  84.00   1.00   13.61    --   14.43   0.00 -30.00  107
  2  \w     -5.00  53.00   1.00   13.61    --   14.43  37.00  30.00   58
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0057829000
_diffrn_orient_matrix_UB_12      0.0183410000
_diffrn_orient_matrix_UB_13      0.0181178000
_diffrn_orient_matrix_UB_21      -0.0357743000
_diffrn_orient_matrix_UB_22      0.0313238000
_diffrn_orient_matrix_UB_23      -0.0081565000
_diffrn_orient_matrix_UB_31      -0.0298766000
_diffrn_orient_matrix_UB_32      -0.0409710000
_diffrn_orient_matrix_UB_33      0.0019037000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0410
_diffrn_reflns_av_unetI/netI     0.0822
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.797
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            24313
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.797
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.429
_diffrn_reflns_theta_min         2.295
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.248
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88015
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.044
_exptl_crystal_description       block
_exptl_crystal_F_000             2376
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.056
_refine_diff_density_min         -0.418
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     728
_refine_ls_number_reflns         14105
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.1240
_refine_ls_R_factor_gt           0.0822
_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^)+(0.1264P)^2^+5.1912P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2192
_refine_ls_wR_factor_ref         0.2545
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8681
_reflns_number_total             14105
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc02063g2.cif
_cod_data_source_block           3e
_cod_depositor_comments
'Adding full bibliography for 1566978--1566986.cif.'
_cod_database_code               1566980
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C63 H84 N4 O5 Mg2 Mn'
_chemical_oxdiff_usercomment     JMP113
_shelx_estimated_absorpt_t_max   0.971
_shelx_estimated_absorpt_t_min   0.936
_reflns_odcompleteness_completeness 98.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(C1)=Sof(H1A)=Sof(C2)=1-FVAR(1)
 Sof(C01N)=Sof(C01X)=Sof(H9)=FVAR(1)
3.a Ternary CH refined with riding coordinates:
 C00R(H00R), C00S(H00S), C00X(H00X), C00Y(H00Y), C012(H012), C015(H015),
 C019(H019), C01I(H01U)
3.b Aromatic/amide H refined with riding coordinates:
 C00G(H00G), C00J(H00J), C00N(H00N), C00Q(H00Q), C00Z(H00Z), C010(H010),
 C014(H014), C016(H016), C017(H017), C01A(H01G), C01B(H01H), C01D(H01L),
 C01F(H01P), C01G(H01Q), C01T(H5), C01X(H9), C020(H020), C022(H022), C023(H023),
  C1(H1A)
3.c Idealised Me refined as rotating group:
 C00V(H00A,H00B,H00C), C013(H01A,H01B,H01C), C018(H01D,H01E,H01F), C01C(H01I,
 H01J,H01K), C01E(H01M,H01N,H01O), C01H(H01R,H01S,H01T), C01K(H01V,H01W,H01X),
 C01L(H01Y,H,HA), C01M(H01Z,HB,HC), C01O(H01,HD,HE), C01P(H1,HF,HG), C01Q(H2,HH,
 HI), C01R(H3,HJ,HK), C01S(H4,HL,HM), C01U(H6,HN,HO), C01V(H7,HP,HQ), C01W(H8,
 HR,HS), C01Y(H10,HT,HU), C01Z(H11,HV,HW), C024(H02A,H02B,H02C), C5(H5A,H5B,H5C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              46338
_shelx_hkl_checksum              65385
_shelx_fab_checksum              70747
_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 1.102
_oxdiff_exptl_absorpt_empirical_full_min 0.914