The reactivity of N-heterocyclic diphospholenes towards iron triad carbonyls
Kazakov, Gennady G.; Druzhkov, Nikolay O.; Rumyantcev, Roman V.; Fukin, Georgy K.; Starikov, Andrey G.; Piskunov, Alexandr V.; Cherkasov, Vladimir K.; New Journal of Chemistry 47 (2023) 5953–5960; doi:10.1039/D3NJ00450C

data_7062342
_publ_section_title
;
 The reactivity of N-heterocyclic diphospholenes towards iron triad
 carbonyls
;
_journal_issue                   12
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              5953
_journal_page_last               5960
_journal_paper_doi               10.1039/D3NJ00450C
_journal_volume                  47
_journal_year                    2023
_chemical_formula_moiety         'C20 H40 Br Mg O5, C4 O4 Co, C4 H8 O'
_chemical_formula_sum            'C28 H48 Br Co Mg O10'
_chemical_formula_weight         707.81
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2023-02-27 deposited with the CCDC.	2023-03-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.5980(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.9480(2)
_cell_length_b                   23.6942(3)
_cell_length_c                   10.69920(10)
_cell_measurement_reflns_used    16039
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.8090
_cell_measurement_theta_min      3.4490
_cell_volume                     3275.96(7)
_computing_cell_refinement       'CrysAlis PRO'
_computing_data_collection       'CrysAlis PRO'
_computing_data_reduction        'CrysAlis PRO'
_computing_molecular_graphics    Mercury
_computing_publication_material  Mercury
_computing_structure_refinement  SHELXL-2014/7
_computing_structure_solution    SHELXT-2014/4
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Xcalibur EOS (CCD)'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_av_unetI/netI     0.0233
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            46071
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.033
_diffrn_reflns_theta_min         3.023
_diffrn_source                   'fine focus sealed tube'
_exptl_absorpt_coefficient_mu    1.813
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.219
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlis PRO 1.171.38.46. Numerical absorption correction based on gaussian
integration over a multifaceted crystal model. Empirical absorption correction
using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.435
_exptl_crystal_description       prism
_exptl_crystal_F_000             1480
_exptl_crystal_size_max          0.780
_exptl_crystal_size_mid          0.530
_exptl_crystal_size_min          0.320
_refine_diff_density_max         1.159
_refine_diff_density_min         -0.505
_refine_diff_density_rms         0.070
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.496(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     371
_refine_ls_number_reflns         9565
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0394
_refine_ls_R_factor_gt           0.0378
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0640P)^2^+3.1500P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0960
_refine_ls_wR_factor_ref         0.0974
_reflns_Friedel_coverage         0.997
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                9233
_reflns_number_total             9565
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj00450c3.cif
_cod_data_source_block           coco4mgbr
_cod_depositor_comments
'Adding full bibliography for 7062340--7062343.cif.'
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               7062342
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.332
_shelx_estimated_absorpt_t_max   0.595
_shelx_res_checksum              97100
_shelx_hkl_checksum              24666