Molybdenum carbonyl assisted reductive tetramerization of CO by activated magnesium(i) compounds: squarate dianion <i>vs.</i> metallo-ketene formation.
Yuvaraj, K.; Mullins, Jeremy C.; Rajeshkumar, Thayalan; Douair, Iskander; Maron, Laurent; Jones, Cameron; Chemical science 14 (2023) 5188–5195; doi:10.1039/d3sc01487h

data_1568938
_publ_section_title
;
 Molybdenum carbonyl assisted reductive tetramerization of CO by activated
 magnesium(i) compounds: squarate dianion <i>vs.</i> metallo-ketene
 formation.
;
_journal_issue                   19
_journal_name_full               'Chemical science'
_journal_page_first              5188
_journal_page_last               5195
_journal_paper_doi               10.1039/d3sc01487h
_journal_volume                  14
_journal_year                    2023
_chemical_formula_sum            'C18 H20 Mo N4 O4'
_chemical_formula_weight         452.32
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2023-03-21 deposited with the CCDC.	2023-04-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.68(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   29.705(6)
_cell_length_b                   9.751(2)
_cell_length_c                   14.098(3)
_cell_measurement_reflns_used    3646
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      2.95
_cell_volume                     3931.6(15)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    xseed
_computing_publication_material  Ciftab
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0389
_diffrn_reflns_av_unetI/netI     0.0229
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            19999
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.491
_diffrn_reflns_theta_min         2.954
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.698
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56021
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.113a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.528
_exptl_crystal_description       block
_exptl_crystal_F_000             1840
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.061
_exptl_crystal_size_min          0.045
_refine_diff_density_max         0.543
_refine_diff_density_min         -0.545
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         3646
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.0297
_refine_ls_R_factor_gt           0.0280
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0304P)^2^+8.7002P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0720
_refine_ls_wR_factor_ref         0.0730
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3441
_reflns_number_total             3646
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc01487h2.cif
_cod_data_source_block           Cj1562
_cod_depositor_comments
'Adding full bibliography for 1568937--1568943.cif.'
_cod_original_cell_volume        3931.5(15)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               1568938
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.953
_shelx_estimated_absorpt_t_max   0.969
_shelx_res_checksum              77194
_shelx_hkl_checksum              27078