Polar Effects in Nitride Coupling Reactions
Sean B. Seymore; Seth N. Brown; Inorganic Chemistry 41 (2002) 462–469; doi:10.1021/ic010844z

data_4317501
_publ_section_title
;
 Polar Effects in Nitride Coupling Reactions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              462
_journal_page_last               469
_journal_paper_doi               10.1021/ic010844z
_journal_volume                  41
_journal_year                    2002
_chemical_formula_moiety         '(HBpz3)Cl2Os(mu-N)Mo(S2CNEt2)3, C6H6'
_chemical_formula_sum            'C30 H46 B Cl2 Mo N10 Os S6'
_chemical_formula_weight         1106.98
_chemical_name_common
;
dichloro[tris(pyrazolyl)borato]osmium(mu-nitrido)
[tris(diethyldithiocarbamate)]molybdenum benzene solvate
;
_chemical_name_systematic
;
?
;
_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     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                74.706(12)
_cell_angle_beta                 88.109(11)
_cell_angle_gamma                70.697(11)
_cell_formula_units_Z            2
_cell_length_a                   11.885(2)
_cell_length_b                   12.372(2)
_cell_length_c                   15.924(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      16.0
_cell_measurement_theta_min      7.0
_cell_volume                     2127.8(6)
_computing_cell_refinement       CAD4
_computing_data_collection       CAD4
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Enraf-Nonius CAD4'
_diffrn_measurement_method       '\w-2\t 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    0.0345
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            7474
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.09
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 160
_diffrn_standards_interval_time  7200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.734
_exptl_absorpt_correction_T_max  0.5699
_exptl_absorpt_correction_T_min  0.4336
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.728
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1098
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.165
_refine_diff_density_min         -1.093
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.036
_refine_ls_goodness_of_fit_obs   1.052
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     509
_refine_ls_number_reflns         7474
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_restrained_S_obs      1.052
_refine_ls_R_factor_all          0.0340
_refine_ls_R_factor_obs          0.0268
_refine_ls_shift/esd_max         -1.641
_refine_ls_shift/esd_mean        0.015
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0347P)^2^+0.6227P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0663
_refine_ls_wR_factor_obs         0.0630
_reflns_number_observed          6605
_reflns_number_total             7474
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic010844z.cif
_cod_data_source_block           osnmo
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0347P)^2^+0.6227P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0347P)^2^+0.6227P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2127.9(5)
_cod_database_code               4317501