Double α,α CH bond insertion into sp<sup>3</sup> CH<sub>2</sub> moiety: synthesis of a Fe carbene bis-hydride dinitrogen complex.
Petit, Julien; Cavaillé, Anthony; Saffon-Merceron, Nathalie; Fustier-Boutignon, Marie; Mézailles, Nicolas; Dalton transactions (Cambridge, England : 2003) 50 (2021) 9554–9559; doi:10.1039/d1dt00610j

data_7707656
_publ_section_title
;
 Double \a,\a CH bond insertion into sp<sup>3</sup> CH<sub>2</sub> moiety:
 synthesis of a Fe carbene bis-hydride dinitrogen complex.
;
_journal_issue                   27
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9554
_journal_page_last               9559
_journal_paper_doi               10.1039/d1dt00610j
_journal_volume                  50
_journal_year                    2021
_chemical_formula_sum            'C43 H68 Cl2 Fe N2 O1.5 P2'
_chemical_formula_weight         825.68
_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   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2021-02-12 deposited with the CCDC.	2021-06-14 downloaded from the CCDC.
;
_cell_angle_alpha                80.9776(13)
_cell_angle_beta                 77.2074(14)
_cell_angle_gamma                86.6279(14)
_cell_formula_units_Z            2
_cell_length_a                   11.0591(4)
_cell_length_b                   11.1758(4)
_cell_length_c                   18.3680(7)
_cell_measurement_reflns_used    9955
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      29.32
_cell_measurement_theta_min      2.86
_cell_volume                     2185.75(14)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      193(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker-AXS D8-Venture CMOS detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0636
_diffrn_reflns_av_unetI/netI     0.0513
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            47842
_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         28.282
_diffrn_reflns_theta_min         2.858
_diffrn_source                   'fine focus sealed tube'
_exptl_absorpt_coefficient_mu    0.576
_exptl_absorpt_correction_T_max  0.7463
_exptl_absorpt_correction_T_min  0.6828
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker-AXS)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.255
_exptl_crystal_description       block
_exptl_crystal_F_000             884
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.492
_refine_diff_density_min         -0.430
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     533
_refine_ls_number_reflns         10829
_refine_ls_number_restraints     214
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0828
_refine_ls_R_factor_gt           0.0471
_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^)+(0.0508P)^2^+1.6838P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1073
_refine_ls_wR_factor_ref         0.1254
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7615
_reflns_number_total             10829
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00610j3.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7707656--7707657.cif.'
_cod_original_formula_sum        'C43 H68 Cl2 Fe N2 O1.50 P2'
_cod_database_code               7707656
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.894
_shelx_estimated_absorpt_t_max   0.919
_shelx_res_checksum              6820