Versatile Reactivity of Phosphagermaallene Tip(t-Bu)Ge═C═PMes* with α-Ethylenic Esters
Ghereg, Dumitru; Ouhsaine, Fatima; Escudié, Jean; Labat, Stéphane; André, Erwan; Miqueu, Karinne; Sotiropoulos, Jean-Marc; Gornitzka, Heinz; Saffon, Nathalie; Organometallics 32 (2013) 1085–; doi:10.1021/om301224t

data_4080092
_publ_section_title
;
 Versatile Reactivity of Phosphagermaallene
 Tip(t-Bu)Ge&#x2550;C&#x2550;PMes* with \a-Ethylenic Esters
;
_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              1085
_journal_paper_doi               10.1021/om301224t
_journal_volume                  32
_journal_year                    2013
_chemical_formula_sum            'C43 H67 Ge O4 P'
_chemical_formula_weight         751.53
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 100.725(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.4119(12)
_cell_length_b                   22.586(2)
_cell_length_c                   18.438(2)
_cell_measurement_reflns_used    2349
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      19.21
_cell_measurement_theta_min      2.19
_cell_volume                     4260.2(8)
_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      193(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.1110
_diffrn_reflns_av_sigmaI/netI    0.1352
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            30046
_diffrn_reflns_theta_full        26.49
_diffrn_reflns_theta_max         26.49
_diffrn_reflns_theta_min         2.10
_exptl_absorpt_coefficient_mu    0.794
_exptl_absorpt_correction_T_max  0.9614
_exptl_absorpt_correction_T_min  0.6923
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker-AXS)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.172
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1616
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.651
_refine_diff_density_min         -0.489
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.979
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     618
_refine_ls_number_reflns         8749
_refine_ls_number_restraints     448
_refine_ls_restrained_S_all      0.983
_refine_ls_R_factor_all          0.1496
_refine_ls_R_factor_gt           0.0592
_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^)+(0.0525P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1096
_refine_ls_wR_factor_ref         0.1411
_reflns_number_gt                4231
_reflns_number_total             8749
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om301224t_si_001.cif
_cod_data_source_block           6
_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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        4260.0(8)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4080092