Insertions of Cyclic and Acyclic Germanium and Tin Heterocarbenoids into Phosphorus‒Chlorine Bonds: Syntheses, Structures, and Reactivities
West, Joseph K.; Stahl, Lothar; Organometallics 31 (2012) 2042–; doi:10.1021/om3000168

data_4076536
_publ_section_title
;
 Insertions of Cyclic and Acyclic Germanium and Tin Heterocarbenoids into
 Phosphorus--Chlorine Bonds: Syntheses, Structures, and Reactivities
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              2042
_journal_paper_doi               10.1021/om3000168
_journal_volume                  31
_journal_year                    2012
_chemical_formula_sum            'C26 H47 Cl2 Ge2 N4 P Si2'
_chemical_formula_weight         718.91
_chemical_name_systematic
;

 ?

;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
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_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                 107.715(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.330(3)
_cell_length_b                   10.0397(16)
_cell_length_c                   22.406(4)
_cell_measurement_reflns_used    8654
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.12
_cell_measurement_theta_min      2.24
_cell_volume                     3713.5(11)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker 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 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0242
_diffrn_reflns_av_sigmaI/netI    0.0195
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            30238
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.77
_exptl_absorpt_coefficient_mu    1.891
_exptl_absorpt_correction_T_max  0.5657
_exptl_absorpt_correction_T_min  0.4901
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.286
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       chunk
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.44
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_exptl_crystal_size_min          0.34
_refine_diff_density_max         0.654
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_refine_ls_extinction_method     none
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_refine_ls_number_parameters     368
_refine_ls_number_reflns         8071
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_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0306
_refine_ls_R_factor_gt           0.0273
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0516P)^2^+1.0046P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0815
_refine_ls_wR_factor_ref         0.0834
_reflns_number_gt                7273
_reflns_number_total             8071
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om3000168_si_001.cif
_cod_data_source_block           5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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        3713.5(10)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4076536