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_1566984
_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 H90 Cr Mg2 N4 O3'
_chemical_formula_sum            'C67 H90 Cr Mg2 N4 O3'
_chemical_formula_weight         1100.04
_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                 99.436(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.3628(2)
_cell_length_b                   12.9497(2)
_cell_length_c                   35.8850(6)
_cell_measurement_reflns_used    6270
_cell_measurement_temperature    173.00(14)
_cell_measurement_theta_max      72.7450
_cell_measurement_theta_min      4.4730
_cell_volume                     7042.50(19)
_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      173.00(14)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4115
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.954
_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     18.00 104.00   1.00   15.20    --   42.36  38.00  30.00   86
  2  \w     86.00 133.00   1.00   73.92    --  105.13 -30.00 -30.00   47
  3  \w     86.00 174.00   1.00   73.92    --  105.13  30.00 -60.00   88
  4  \w     73.00 178.00   1.00   73.92    --  105.13  77.00 -30.00  105
  5  \w     28.00 109.00   1.00   73.92    --  105.13 -95.00 -90.00   81
  6  \w     29.00  64.00   1.00   73.92    --  105.13 -30.00 -30.00   35
  7  \w      6.00  98.00   1.00   15.20    --   42.36-125.00-120.00   92
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0708528000
_diffrn_orient_matrix_UB_12      0.0482582000
_diffrn_orient_matrix_UB_13      0.0204516000
_diffrn_orient_matrix_UB_21      -0.0628274000
_diffrn_orient_matrix_UB_22      -0.0901498000
_diffrn_orient_matrix_UB_23      -0.0133587000
_diffrn_orient_matrix_UB_31      0.0369898000
_diffrn_orient_matrix_UB_32      -0.0607422000
_diffrn_orient_matrix_UB_33      0.0360194000
_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  0.0362
_diffrn_reflns_av_unetI/netI     0.0515
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            23388
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.375
_diffrn_reflns_theta_min         3.515
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.829
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97620
_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 orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.038
_exptl_crystal_description       block
_exptl_crystal_F_000             2368
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.343
_refine_diff_density_min         -0.517
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     727
_refine_ls_number_reflns         13503
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0724
_refine_ls_R_factor_gt           0.0517
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0844P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1388
_refine_ls_wR_factor_ref         0.1558
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9836
_reflns_number_total             13503
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc02063g2.cif
_cod_data_source_block           3d
_cod_depositor_comments
'Adding full bibliography for 1566978--1566986.cif.'
_cod_database_code               1566984
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C67 H91 Cr1 Mg2 N4 O3'
_chemical_oxdiff_usercomment     JMP-084
_shelx_estimated_absorpt_t_max   0.810
_shelx_estimated_absorpt_t_min   0.771
_reflns_odcompleteness_completeness 98.48
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_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. Uiso/Uaniso restraints and constraints
C1 \\sim C01U \\sim C2 \\sim C01S: within 1A with sigma of 0.01 and sigma for
terminal atoms of 0.01 within 1A
3. Others
 Sof(C1)=Sof(H1A)=Sof(C2)=1-FVAR(1)
 Sof(C01S)=Sof(H6)=Sof(C01U)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C00U(H00U), C00V(H00V), C00W(H00W), C00Z(H00Z), C010(H010), C015(H015),
 C01B(H01H), C01J(H01W)
4.b Aromatic/amide H refined with riding coordinates:
 C00I(H00I), C00M(H00M), C00N(H00N), C00S(H00S), C00X(H00X), C00Y(H00Y),
 C011(H011), C014(H014), C017(H017), C018(H018), C019(H019), C01A(H01G),
 C01E(H01L), C01F(H01M), C01M(H01), C01S(H6), C01T(H7), C01V(H8), C01X(H10),
 C01Y(H11), C022(H022), C1(H1A)
4.c Idealised Me refined as rotating group:
 C013(H01A,H01B,H01C), C016(H01D,H01E,H01F), C01D(H01I,H01J,H01K), C01G(H01N,
 H01O,H01P), C01H(H01Q,H01R,H01S), C01I(H01T,H01U,H01V), C01K(H01X,H01Y,H),
 C01L(H01Z,HA,HB), C01N(H1,HC,HD), C01O(H2,HE,HF), C01P(H3,HG,HH), C01Q(H4,HI,
 HJ), C01R(H5,HK,HL), C01W(H9,HM,HN), C01Z(H12,HO,HP), C020(H02A,H02B,H02C),
 C021(H02D,H02E,H02F), C023(H02G,H02H,H02I), C024(H02J,H02K,H02L), C025(H02M,
 H02N,H02O)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 198 electrons were 
found in a volume of 1230\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
0.8[C6H14] per Asymmetric Unit 
which account for 200 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              18660
_shelx_hkl_checksum              13598
_shelx_fab_checksum              87442
_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 1.142
_oxdiff_exptl_absorpt_empirical_full_min 0.908