Transition Metal Complexes of a “Half-Parent” Phosphasilene Adduct Representing Silylene→Phosphinidene→Metal Complexes
Hansen, Kerstin; Szilvási, Tibor; Blom, Burgert; Driess, Matthias; Organometallics 34 (2015) 5703–; doi:10.1021/acs.organomet.5b00772

data_4087982
_publ_section_title
;
 Transition Metal Complexes of a &#x201C;Half-Parent&#x201D; Phosphasilene
 Adduct Representing Silylene\\rightarrow Phosphinidene\\rightarrow Metal
 Complexes
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              5703
_journal_paper_doi               10.1021/acs.organomet.5b00772
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         '2(C41 H51 Mo N4 O5 P Si), 3(C7 H8)'
_chemical_formula_sum            'C103 H126 Mo2 N8 O10 P2 Si2'
_chemical_formula_weight         1946.12
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
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;
_cell_angle_alpha                90.00
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_cell_length_a                   15.9982(13)
_cell_length_b                   20.0928(8)
_cell_length_c                   17.7845(10)
_cell_measurement_reflns_used    2744
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      73.6450
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_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2717
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'four-circle diffractometer'
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_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1091
_diffrn_reflns_av_sigmaI/netI    0.1263
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            21070
_diffrn_reflns_theta_full        67.50
_diffrn_reflns_theta_max         67.50
_diffrn_reflns_theta_min         3.04
_diffrn_source                   'sealed X-ray tube'
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_exptl_absorpt_coefficient_mu    2.954
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;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.245
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2044
_exptl_crystal_size_max          0.28
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_refine_diff_density_max         1.122
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_refine_ls_extinction_method     none
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_refine_ls_number_parameters     618
_refine_ls_number_reflns         9344
_refine_ls_number_restraints     187
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.1237
_refine_ls_R_factor_gt           0.0741
_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^)+(0.0531P)^2^+1.9921P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1612
_refine_ls_wR_factor_ref         0.1936
_reflns_number_gt                5822
_reflns_number_total             9344
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5b00772_si_002.cif
_cod_data_source_block           p21c
_cod_original_cell_volume        5191.5(6)
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4087982