Low-Valent Aminopyridinato Chromium Methyl Complexes via Reductive Alkylation and via Oxidative Addition of Iodomethane by a Cr–Cr Quintuple Bond
Noor, Awal; Schwarz, Stefan; Kempe, Rhett; Organometallics 34 (2015) 2122–; doi:10.1021/om501230g

data_4085498
_publ_section_title
;
 Low-Valent Aminopyridinato Chromium Methyl Complexes via Reductive
 Alkylation and via Oxidative Addition of Iodomethane by a Cr--Cr
 Quintuple Bond
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              2122
_journal_paper_doi               10.1021/om501230g
_journal_volume                  34
_journal_year                    2015
_chemical_formula_sum            'C65 H77 Cr2 I N4'
_chemical_formula_weight         1145.21
_chemical_name_common            'Compound 9'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                65.129(5)
_cell_angle_beta                 89.534(6)
_cell_angle_gamma                69.427(5)
_cell_formula_units_Z            1
_cell_length_a                   10.4779(8)
_cell_length_b                   11.8984(8)
_cell_length_c                   13.6997(9)
_cell_measurement_reflns_used    all
_cell_measurement_temperature    133(2)
_cell_volume                     1431.0(2)
_computing_cell_refinement       X-AREA-STOE
_computing_data_collection       X-AREA-STOE
_computing_data_reduction        X-AREA-STOE
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-97
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  STOE-IPDSII
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1969
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5408
_diffrn_reflns_theta_full        25.77
_diffrn_reflns_theta_max         25.77
_diffrn_reflns_theta_min         1.66
_exptl_absorpt_coefficient_mu    0.962
_exptl_absorpt_correction_T_max  0.9438
_exptl_absorpt_correction_T_min  0.8440
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             596
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.723
_refine_diff_density_min         -0.596
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.795
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     332
_refine_ls_number_reflns         5408
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.795
_refine_ls_R_factor_all          0.1391
_refine_ls_R_factor_gt           0.0595
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0355P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1026
_refine_ls_wR_factor_ref         0.1205
_reflns_number_gt                2654
_reflns_number_total             5408
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om501230g_si_001.cif
_cod_data_source_block           k922a
_cod_depositor_comments
'Adding full bibliography for 4085493--4085498.cif.'
_cod_original_cell_volume        1430.98(17)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4085498
_cell_measurement_2theta_min     3.32
_cell_measurement_2theta_max     52.04