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_7707657
_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            'C92 H148 Fe2 N6 O4.5 P4'
_chemical_formula_weight         1645.74
_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 space'
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-02-12 deposited with the CCDC.	2021-06-14 downloaded from the CCDC.
;
_cell_angle_alpha                104.573(2)
_cell_angle_beta                 95.791(3)
_cell_angle_gamma                98.177(2)
_cell_formula_units_Z            2
_cell_length_a                   13.3756(11)
_cell_length_b                   15.4294(11)
_cell_length_c                   22.9638(19)
_cell_measurement_reflns_used    9911
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      25.16
_cell_measurement_theta_min      2.75
_cell_volume                     4493.7(6)
_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-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT (Sheldrick 2015)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker kappa APEX-II CCD Quazar'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0858
_diffrn_reflns_av_unetI/netI     0.0783
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            100492
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.373
_diffrn_reflns_theta_min         1.385
_diffrn_source                   'Incoatec microfocus sealed tube'
_exptl_absorpt_coefficient_mu    0.447
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.7014
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker-AXS)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.216
_exptl_crystal_description       block
_exptl_crystal_F_000             1780
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.130
_refine_diff_density_max         0.824
_refine_diff_density_min         -0.640
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1200
_refine_ls_number_reflns         18321
_refine_ls_number_restraints     888
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.1016
_refine_ls_R_factor_gt           0.0570
_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^)+(0.0703P)^2^+3.3919P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1358
_refine_ls_wR_factor_ref         0.1567
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12115
_reflns_number_total             18321
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00610j3.cif
_cod_data_source_block           3d
_cod_depositor_comments
'Adding full bibliography for 7707656--7707657.cif.'
_cod_original_formula_sum        'C92 H148 Fe2 N6 O4.50 P4'
_cod_database_code               7707657
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.916
_shelx_estimated_absorpt_t_max   0.944
_shelx_res_checksum              767