Synthesis and Reactivity of Molybdenum(IV) Complexes with Alkyl and Aryl Isocyanides
Ison, Elon A.; Ortiz, Carlos O.; Abboud, Khalil; Boncella, James M.; Organometallics 24 (2005) 6310–; doi:10.1021/om0502436

data_4075883
_publ_section_title
;
 Synthesis and Reactivity of Molybdenum(IV) Complexes with Alkyl and Aryl
 Isocyanides
;
_journal_issue                   26
_journal_name_full               Organometallics
_journal_page_first              6310
_journal_paper_doi               10.1021/om0502436
_journal_volume                  24
_journal_year                    2005
_chemical_formula_sum            'C33 H54 Mo N6 Si2'
_chemical_formula_weight         686.94
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.4614(6)
_cell_length_b                   18.571(1)
_cell_length_c                   19.715(1)
_cell_measurement_temperature    173(2)
_cell_volume                     3830.2(4)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0841
_diffrn_reflns_av_sigmaI/netI    0.1219
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            27445
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.07
_exptl_absorpt_coefficient_mu    0.433
_exptl_absorpt_correction_T_max  0.966
_exptl_absorpt_correction_T_min  0.786
_exptl_absorpt_correction_type   'Empirical (SADABS, Blessing 1995)'
_exptl_crystal_colour            Purple
_exptl_crystal_density_diffrn    1.191
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needles
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          .34
_exptl_crystal_size_mid          .08
_exptl_crystal_size_min          .08
_refine_diff_density_max         0.563
_refine_diff_density_min         -0.455
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(4)
_refine_ls_extinction_coef       0.00054(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.910
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     431
_refine_ls_number_reflns         8793
_refine_ls_number_restraints     61
_refine_ls_restrained_S_all      0.908
_refine_ls_R_factor_all          0.1086
_refine_ls_R_factor_gt           0.0483
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0433P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0854
_refine_ls_wR_factor_ref         0.0992
_reflns_number_gt                5197
_reflns_number_total             8793
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0502436si20050331_045034.cif
_cod_data_source_block           compound_3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        3830.1(4)
_cod_original_sg_symbol_H-M      P2(1)2(1)2(1)
_cod_database_code               4075883