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_1566985
_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         'C63 H84 Fe Mg2 N4 O5, 2(C7 H8)'
_chemical_formula_sum            'C77 H100 Fe Mg2 N4 O5'
_chemical_formula_weight         1266.07
_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   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                99.136(4)
_cell_angle_beta                 97.078(4)
_cell_angle_gamma                112.627(6)
_cell_formula_units_Z            2
_cell_length_a                   13.3957(10)
_cell_length_b                   13.4353(8)
_cell_length_c                   22.6744(8)
_cell_measurement_reflns_used    6849
_cell_measurement_temperature    173.00(14)
_cell_measurement_theta_max      28.1240
_cell_measurement_theta_min      2.7200
_cell_volume                     3642.1(4)
_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 16.0382
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.799
_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     -2.00  82.00   1.00   42.50    --   14.43  57.00-180.00   84
  2  \w    -53.00  40.00   1.00   42.50    --   14.43 -77.00 -90.00   93
  3  \w    -11.00  82.00   1.00   42.50    --   14.43  77.00  30.00   93
;
_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      0.0199965000
_diffrn_orient_matrix_UB_12      0.0211332000
_diffrn_orient_matrix_UB_13      0.0318674000
_diffrn_orient_matrix_UB_21      -0.0400238000
_diffrn_orient_matrix_UB_22      0.0223407000
_diffrn_orient_matrix_UB_23      0.0011948000
_diffrn_orient_matrix_UB_31      -0.0378070000
_diffrn_orient_matrix_UB_32      -0.0500030000
_diffrn_orient_matrix_UB_33      0.0054524000
_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  0.0288
_diffrn_reflns_av_unetI/netI     0.0624
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.799
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            20927
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.799
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.221
_diffrn_reflns_theta_min         2.576
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.275
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85621
_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 green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.154
_exptl_crystal_description       block
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.167
_refine_diff_density_min         -0.599
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     922
_refine_ls_number_reflns         14369
_refine_ls_number_restraints     180
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.1270
_refine_ls_R_factor_gt           0.0980
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1080P)^2^+19.3278P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3006
_refine_ls_wR_factor_ref         0.3168
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10076
_reflns_number_total             14369
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc02063g2.cif
_cod_data_source_block           3c
_cod_depositor_comments
'Adding full bibliography for 1566978--1566986.cif.'
_cod_database_code               1566985
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C63 H84 N4 Fe1 Mg2'
_shelx_estimated_absorpt_t_max   0.978
_shelx_estimated_absorpt_t_min   0.952
_reflns_odcompleteness_completeness 98.96
_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. Rigid body (RIGU) restrains
 C3, C1, C027, C7, C02A, C026, C6, C9, H9A, C3A, C1A, C6A, C10, C02B, C7A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C029, C2, C025, C028, C0AA, C1AA, C024, C0, C2A, C4, C8, C0AB, C1AB, C5
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Others
 Sof(C0)=Sof(H0A)=Sof(H0B)=Sof(H0C)=Sof(C2A)=Sof(C4)=Sof(H4A)=Sof(C8)=Sof(H8A)=
 Sof(C0AB)=Sof(H0AB)=Sof(C1AB)=Sof(H1AB)=Sof(C5)=Sof(H5A)=1-FVAR(1)
 Sof(C029)=Sof(H02J)=Sof(H02K)=Sof(H02L)=Sof(C2)=Sof(C025)=Sof(H025)=Sof(C028)=
 Sof(H028)=Sof(C0AA)=Sof(H0AA)=Sof(C1AA)=Sof(H1AA)=Sof(C024)=Sof(H024)=FVAR(1)
 Sof(C9)=Sof(H9A)=Sof(C3A)=Sof(C1A)=Sof(H1AC)=Sof(C6A)=Sof(H6AA)=Sof(H6AB)=
 Sof(H6AC)=Sof(C10)=Sof(H10A)=Sof(C02B)=Sof(H02N)=Sof(C7A)=Sof(H7AA)=1-FVAR(2)
 Sof(C3)=Sof(C1)=Sof(H1A)=Sof(C027)=Sof(H027)=Sof(C7)=Sof(H7A)=Sof(C02A)=
 Sof(H02M)=Sof(C026)=Sof(H026)=Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(H6C)=FVAR(2)
4.a Ternary CH refined with riding coordinates:
 C00H(H00H), C00I(H00I), C00M(H00M), C00Y(H00Y), C018(H018), C019(H019),
 C01F(H01Q), C01I(H01V)
4.b Aromatic/amide H refined with riding coordinates:
 C00C(H00C), C00J(H00J), C00O(H00O), C00W(H00W), C00Z(H00Z), C010(H010),
 C011(H011), C012(H012), C015(H015), C01D(H01M), C01H(H01U), C01J(H01W),
 C01M(H01), C01N(H1), C01P(H3), C1(H1A), C027(H027), C7(H7A), C02A(H02M),
 C026(H026), C025(H025), C028(H028), C0AA(H0AA), C1AA(H1AA), C024(H024),
 C4(H4A), C8(H8A), C0AB(H0AB), C1AB(H1AB), C5(H5A), C9(H9A), C1A(H1AC),
 C10(H10A), C02B(H02N), C7A(H7AA)
4.c Fitted hexagon refined as free rotating group:
 C3(C1,C027,C7,C02A,C026), C2(C025,C028,C0AA,C1AA,C024), C2A(C4,C8,C0AB,C1AB,C5)
4.d Idealised Me refined as rotating group:
 C014(H01A,H01B,H01C), C016(H01D,H01E,H01F), C01B(H01G,H01H,H01I), C01C(H01J,
 H01K,H01L), C01E(H01N,H01O,H01P), C01G(H01R,H01S,H01T), C01K(H01X,H01Y,H),
 C01L(H01Z,HA,HB), C01O(H2,HC,HD), C01Q(H4,HE,HF), C01R(H5,HG,HH), C01S(H6,HI,
 HJ), C01T(H7,HK,HL), C01U(H8,HM,HN), C01V(H9,HO,HP), C01W(H10,HQ,HR), C01Y(H11,
 HS,HT), C021(H02A,H02B,H02C), C022(H02D,H02E,H02F), C023(H02G,H02H,H02I),
 C029(H02J,H02K,H02L), C6(H6A,H6B,H6C), C0(H0A,H0B,H0C), C6A(H6AA,H6AB,H6AC)
;
_shelx_res_checksum              69591
_shelx_hkl_checksum              60133
_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 1.136
_oxdiff_exptl_absorpt_empirical_full_min 0.892