Sterically controlled reductive oligomerisations of CO by activated magnesium(i) compounds: deltate vs. ethenediolate formation
Yuvaraj, K.; Douair, Iskander; Jones, Dafydd D. L.; Maron, Laurent; Jones, Cameron; Chemical Science 11 (2020) 3516–3522; doi:10.1039/D0SC00836B

data_1557552
_publ_section_title
;
 Sterically controlled reductive oligomerisations of CO by activated
 magnesium(i) compounds: deltate vs. ethenediolate formation
;
_journal_issue                   13
_journal_name_full               'Chemical Science'
_journal_page_first              3516
_journal_page_last               3522
_journal_paper_doi               10.1039/D0SC00836B
_journal_volume                  11
_journal_year                    2020
_chemical_formula_sum            'C134 H184 Mg4 N12 O12'
_chemical_formula_weight         2252.16
_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   geom
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2020-02-12 deposited with the CCDC.	2020-03-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.08(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.480(3)
_cell_length_b                   15.114(3)
_cell_length_c                   27.505(6)
_cell_measurement_reflns_used    11188
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.20
_cell_measurement_theta_min      2.96
_cell_volume                     6268(2)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'Blu-Ice (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_molecular_graphics    X-Seed
_computing_publication_material  CifTAB
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.7109
_diffrn_reflns_av_R_equivalents  0.1941
_diffrn_reflns_av_unetI/netI     0.1088
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            71723
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.199
_diffrn_reflns_theta_max         25.199
_diffrn_reflns_theta_min         2.961
_diffrn_source                   'Australian Synchrotron'
_exptl_absorpt_coefficient_mu    0.094
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.991
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   XDS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.193
_exptl_crystal_description       block
_exptl_crystal_F_000             2432
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.080
_platon_squeeze_details
;
 4 molecules of heavily disordered THF were 
  located in the asymmetric unit, but all ttempts to model their disorder
  were unsatisfactory. As a result the SQUEEZE program was used to remove
  their contribution to the structure factors, and the structure refined
  including the contribution of the THF molecules to the empirical formula
  and F(000).
;
_refine_diff_density_max         0.472
_refine_diff_density_min         -0.318
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     564
_refine_ls_number_reflns         11188
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.2102
_refine_ls_R_factor_gt           0.1035
_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^)+(0.1911P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2942
_refine_ls_wR_factor_ref         0.3675
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4302
_reflns_number_total             11188
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc00836b2.cif
_cod_data_source_block           Cj1405
_cod_depositor_comments
;Adding full bibliography for 1557543--1557552.cif.

 Adding full bibliography for 1557543--1557552.cif.
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1557552
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.990
_shelx_estimated_absorpt_t_max   0.993
_shelx_res_checksum              73538
_shelx_fab_checksum              78327
_platon_squeeze_void_probe_radius 1.20