Multiple coupling of silanes with imido complexes of Mo.
Khalimon, Andrey Y.; McLeod, Nicolas A.; Ignatov, Stanislav K.; Okhapkin, Andrey I.; Kuzmina, Lyudmila G.; Howard, Judith A. K.; Nikonov, Georgii I.; Dalton transactions (Cambridge, England : 2003) 43 (2014) 8446–8453; doi:10.1039/c4dt00154k

data_7029876
_publ_section_title
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 Multiple coupling of silanes with imido complexes of Mo.
;
_journal_issue                   22
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8446
_journal_page_last               8453
_journal_paper_doi               10.1039/c4dt00154k
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C32 H56 Mo N2 P2 Si3'
_chemical_formula_sum            'C32 H56 Mo N2 P2 Si3'
_chemical_formula_weight         710.94
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-02-28
_audit_creation_method
;
Olex2 1.2
(compiled 2014.02.17 svn.r2891 for OlexSys, GUI svn.r4773)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 100.687(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.893(3)
_cell_length_b                   22.133(7)
_cell_length_c                   15.524(5)
_cell_measurement_temperature    123(2)
_cell_volume                     3678(2)
_computing_cell_refinement       'SAINT (Bruker, 2008)'
_computing_data_collection       'APEX2 (Bruker, 2008)'
_computing_data_reduction        'SAINT (Bruker, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123.15
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.4172
_diffrn_reflns_av_unetI/netI     0.4581
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            24037
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.62
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.565
_exptl_absorpt_correction_T_max  0.9562
_exptl_absorpt_correction_T_min  0.8858
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.284
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.919
_refine_diff_density_min         -0.887
_refine_diff_density_rms         0.144
_refine_ls_extinction_coef       0.094(4)
_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   0.733
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     362
_refine_ls_number_reflns         8295
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.733
_refine_ls_R_factor_all          0.3144
_refine_ls_R_factor_gt           0.0960
_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^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1983
_refine_ls_wR_factor_ref         0.2576
_reflns_number_gt                2257
_reflns_number_total             8295
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt00154k2.cif
_cod_data_source_block           p21n
_cod_depositor_comments          'Adding full bibliography for 7029876.cif.'
_cod_database_code               7029876
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: C4B(0.6) H4BA(0.6) H4BB(0.6) H4BC(0.6) C4BA(0.4) H4BD(0.4)
 H4BE(0.4) H4BF(0.4)
 Fixed Uiso: H3(0.0632) H1A(0.0771) H1B(0.07347) H2(0.06386)
3.a Everything fixed:
 H1A, H1B, H2
3.b Riding coordinates:
 Mo1(H), Si3(H3)
3.c Me refined with riding coordinates:
 C2A(H2AA,H2AB,H2AC), C3A(H3AA,H3AB,H3AC), C4A(H4AA,H4AB,H4AC), C2B(H2BA,H2BB,
 H2BC), C3B(H3BA,H3BB,H3BC), C4B(H4BA,H4BB,H4BC), C4BA(H4BD,H4BE,H4BF),
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,
 H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C)
3.d Aromatic/amide H refined with riding coordinates:
 C2(H2A), C3(H3A), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18)
;