Avenue to phosphaalkenes from Ph<sub>3</sub>GePCO.
Szkop, Kevin M.; Jupp, Andrew R.; Razumkov, Hlib; Stephan, Douglas W.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 885–890; doi:10.1039/c9dt04590b

data_7702970
_publ_section_title
;
 Avenue to phosphaalkenes from Ph<sub>3</sub>GePCO.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              885
_journal_page_last               890
_journal_paper_doi               10.1039/c9dt04590b
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C45 H48 Ge O P2 Si'
_chemical_formula_sum            'C45 H48 Ge O P2 Si'
_chemical_formula_weight         767.45
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-12-08
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-12-12 deposited with the CCDC.	2019-12-13 downloaded from the CCDC.
;
_cell_angle_alpha                113.791(3)
_cell_angle_beta                 94.049(3)
_cell_angle_gamma                110.342(3)
_cell_formula_units_Z            4
_cell_length_a                   16.0049(15)
_cell_length_b                   16.340(2)
_cell_length_c                   18.646(2)
_cell_measurement_reflns_used    9353
_cell_measurement_temperature    149(2)
_cell_measurement_theta_max      27.30
_cell_measurement_theta_min      2.20
_cell_volume                     4055.4(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      149.53
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0891
_diffrn_reflns_av_unetI/netI     0.0783
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            77585
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.437
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.897
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.257
_exptl_crystal_description       shard
_exptl_crystal_F_000             1608
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.369
_refine_diff_density_min         -0.403
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.988
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     913
_refine_ls_number_reflns         14251
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.988
_refine_ls_R_factor_all          0.0931
_refine_ls_R_factor_gt           0.0417
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0462P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0892
_refine_ls_wR_factor_ref         0.1067
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8771
_reflns_number_total             14251
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04590b2.cif
_cod_data_source_block           kev013_0m
_cod_depositor_comments
'Adding full bibliography for 7702969--7702970.cif.'
_cod_database_code               7702970
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.948
_shelx_estimated_absorpt_t_min   0.892
_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.a Aromatic/amide H refined with riding coordinates:
 C55(H55), C32(H32), C82(H82), C88(H88), C84(H84), C0AA(H0AA), C11(H11),
 C38(H38), C23(H23), C57(H57), C71(H71), C26(H26), C67(H67), C20(H20), C17(H17),
  C63(H63), C59(H59), C61(H61), C21(H21), C58(H58), C65(H65), C34(H34),
 C25(H25), C15(H15), C37(H37), C85(H85), C64(H64), C40(H40), C74(H74), C73(H73),
  C6AA(H6AA), C56(H56), C24(H24), C68(H68), C12(H12), C44(H44), C36(H36),
 C13(H13), C28(H28), C87(H87), C31(H31), C78(H78), C62(H62), C18(H18), C75(H75),
  C30(H30), C19(H19), C35(H35), C81(H81), C86(H86), C29(H29), C69(H69),
 C76(H76), C70(H70), C41(H41), C42(H42), C14(H14), C43(H43), C79(H79), C80(H80)
2.b Idealised Me refined as rotating group:
 C47(H47A,H47B,H47C), C52(H52A,H52B,H52C), C51(H51A,H51B,H51C), C7(H7A,H7B,
 H7C), C53(H53A,H53B,H53C), C9(H9A,H9B,H9C), C5(H5A,H5B,H5C), C8(H8A,H8B,H8C),
 C49(H49A,H49B,H49C), C48(H48A,H48B,H48C), C4(H4A,H4B,H4C), C3(H3A,H3B,H3C)
;
_shelx_res_checksum              35489
_olex2_submission_special_instructions 'No special instructions were received'