Synthesis and Reversible Reductive Coupling of Cationic, Dinitrogen-Derived Diazoalkane Complexes
John J. Curley; Tetsuro Murahashi; Christopher C. Cummins; Inorganic Chemistry 48 (2009) 7181–7193; doi:10.1021/ic900495s

data_4302825
_publ_contact_author_address
;Department of Chemistry
Massachusetts Institute of Technology
77 Massachusetts Avenue
Room 6-325
Cambridge, MA
02139
;
_publ_contact_author_email       ccummins@mit.edu
_publ_contact_author_name        'Christopher C. Cummins'
_publ_section_title
;
Synthesis and Reversible Reductive Coupling of Cationic, Dinitrogen-Derived
Diazoalkane Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7181
_journal_page_last               7193
_journal_paper_doi               10.1021/ic900495s
_journal_volume                  48
_journal_year                    2009
_chemical_absolute_configuration ad
_chemical_formula_sum            'C102 H152 Mo2 N10 O4'
_chemical_formula_weight         1774.22
_chemical_name_common            '[PhC(H)NNMo(N[t-Bu]Ar)3]2'
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 106.209(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   28.188(2)
_cell_length_b                   10.3537(7)
_cell_length_c                   17.5606(14)
_cell_measurement_reflns_used    5650
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.18
_cell_measurement_theta_min      2.32
_cell_volume                     4921.3(6)
_computing_cell_refinement       'SAINT 5 (Bruker-AXS, 2003)'
_computing_data_collection       'SMART 5 (Bruker-AXS, 2003)'
_computing_data_reduction        'SAINT 5 (Bruker-AXS, 2003)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker Smart APEX CCD'
_diffrn_measurement_method       'omega and phi scans'
_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    0.0535
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            12137
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.11
_exptl_absorpt_coefficient_mu    0.309
_exptl_absorpt_correction_T_max  0.9787
_exptl_absorpt_correction_T_min  0.9610
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.197
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1900
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.394
_refine_diff_density_min         -0.487
_refine_diff_density_rms         0.078
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.05(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     550
_refine_ls_number_reflns         12137
_refine_ls_number_restraints     82
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0553
_refine_ls_R_factor_gt           0.0446
_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^)+(0.0587P)^2^+2.1140P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1028
_refine_ls_wR_factor_ref         0.1091
_reflns_number_gt                10682
_reflns_number_total             12137
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic900495s_si_001_1.cif
_cod_data_source_block           '[1-H]2'
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        4921.4(6)
_cod_original_sg_symbol_H-M      'C 2'
_cod_database_code               4302825