A novel synthesis of metallogermacyclopropane and molybdenum bis(iminophosphorano)carbene complexes from bisgermavinylidene
Leung, Wing-Por; So, Cheuk-Wai; Wang, Jin-Zhi; Mak, Thomas C. W.; Chemical Communications (Cambridge, United Kingdom)  (2003) 248–249; doi:10.1039/b210598e

data_7113521
_publ_section_title
;
 A novel synthesis of metallogermacyclopropane and molybdenum
 bis(iminophosphorano)carbene complexes from bisgermavinylidene
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   2
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              248
_journal_page_last               249
_journal_paper_doi               10.1039/b210598e
_journal_year                    2003
_chemical_formula_sum            'C42 H59 Mo N2 O5 P2 Si2'
_chemical_formula_weight         885.97
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                98.922(2)
_cell_angle_beta                 95.369(2)
_cell_angle_gamma                110.193(2)
_cell_formula_units_Z            2
_cell_length_a                   11.1278(11)
_cell_length_b                   14.2454(13)
_cell_length_c                   16.2005(15)
_cell_measurement_temperature    293(2)
_cell_volume                     2350.9(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_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  0.0158
_diffrn_reflns_av_sigmaI/netI    0.0292
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            15832
_diffrn_reflns_theta_full        28.03
_diffrn_reflns_theta_max         28.03
_diffrn_reflns_theta_min         1.55
_exptl_absorpt_coefficient_mu    0.439
_exptl_absorpt_correction_T_max  0.7634
_exptl_absorpt_correction_T_min  0.5588
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_density_diffrn    1.252
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             930
_exptl_crystal_size_max          1.50
_exptl_crystal_size_mid          0.72
_exptl_crystal_size_min          0.65
_refine_diff_density_max         3.783
_refine_diff_density_min         -0.340
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         11098
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.0429
_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^)+(0.0772P)^2^+1.3708P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1219
_refine_ls_wR_factor_ref         0.1282
_reflns_number_gt                9410
_reflns_number_total             11098
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             7103937
_cod_data_source_file            b210598e.txt
_cod_data_source_block           scw178
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      p-1
_cod_database_code               7113521