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_1566978
_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         'C64 H84 Cr Mg2 N4 O6, C7 H8'
_chemical_formula_sum            'C71 H92 Cr Mg2 N4 O6'
_chemical_formula_weight         1198.10
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2021-10-15 deposited with the CCDC.	2022-05-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   35.2188(4)
_cell_length_b                   15.39140(16)
_cell_length_c                   12.77462(11)
_cell_measurement_reflns_used    6951
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      73.5620
_cell_measurement_theta_min      4.2660
_cell_volume                     6924.70(12)
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'CIFTAB-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 10.3745
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type  'Agilent Xcalibur PX Ultra A'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0276
_diffrn_reflns_av_unetI/netI     0.0426
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            14191
_diffrn_reflns_point_group_measured_fraction_full 0.731
_diffrn_reflns_point_group_measured_fraction_max 0.697
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.759
_diffrn_reflns_theta_min         3.814
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.934
_exptl_absorpt_correction_T_max  0.904
_exptl_absorpt_correction_T_min  0.660
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) 
(compiled Aug 13 2014,18:06:01) 
Analytical numeric absorption correction using a multifaceted crystal 
model based on expressions derived by R.C. Clark & J.S. Reid. 
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) 
Empirical absorption correction using spherical harmonics, 
implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.149
_exptl_crystal_description       plates
_exptl_crystal_F_000             2568
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.240
_refine_diff_density_min         -0.259
_refine_diff_density_rms         0.036
_refine_ls_abs_structure_details
; 
 Flack x determined using 2322 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   -0.002(4)
_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     797
_refine_ls_number_reflns         9749
_refine_ls_number_restraints     56
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0376
_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^)+(0.0536P)^2^+0.5382P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0931
_refine_ls_wR_factor_ref         0.0978
_reflns_Friedel_coverage         0.387
_reflns_Friedel_fraction_full    0.449
_reflns_Friedel_fraction_max     0.408
_reflns_number_gt                8954
_reflns_number_total             9749
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc02063g2.cif
_cod_data_source_block           3a
_cod_depositor_comments
'Adding full bibliography for 1566978--1566986.cif.'
_cod_database_code               1566978
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              47970
_shelx_hkl_checksum              7484