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_7702969
_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         'C49 H58 Ge O2 P2 Si'
_chemical_formula_sum            'C49 H58 Ge O2 P2 Si'
_chemical_formula_weight         841.57
_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             2019-12-11
_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                109.25(3)
_cell_angle_beta                 93.811(19)
_cell_angle_gamma                105.368(13)
_cell_formula_units_Z            2
_cell_length_a                   12.244(9)
_cell_length_b                   13.196(9)
_cell_length_c                   16.490(12)
_cell_measurement_reflns_used    5815
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      23.53
_cell_measurement_theta_min      2.25
_cell_volume                     2391(3)
_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      150
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.951
_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  0.0753
_diffrn_reflns_av_unetI/netI     0.1456
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            26886
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.631
_diffrn_reflns_theta_min         2.254
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.768
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6939
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0799 before and 0.0630 after correction.
The Ratio of minimum to maximum transmission is 0.9307.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.169
_exptl_crystal_description       plate
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.06
_platon_squeeze_details
;
The unit cell contains 2 (C2H5)2O molecules that have been treated as 
	a diffuse contribution to the overall scattering with specific atom positions by SQUEEZE/PLATON.
;
_refine_diff_density_max         0.385
_refine_diff_density_min         -0.606
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.937
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     457
_refine_ls_number_reflns         10562
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.937
_refine_ls_R_factor_all          0.1211
_refine_ls_R_factor_gt           0.0555
_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^)+(0.0455P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1058
_refine_ls_wR_factor_ref         0.1201
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5784
_reflns_number_total             10562
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04590b2.cif
_cod_data_source_block           kev005_0m_a_sqd
_cod_depositor_comments
'Adding full bibliography for 7702969--7702970.cif.'
_cod_database_code               7702969
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.955
_shelx_estimated_absorpt_t_min   0.874
_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:
 C11(H11), C12(H12), C13(H13), C14(H14), C15(H15), C17(H17), C18(H18),
 C19(H19), C20(H20), C21(H21), C23(H23), C24(H24), C25(H25), C26(H26), C27(H27),
  C29(H29), C30(H30), C31(H31), C32(H32), C33(H33), C35(H35), C36(H36),
 C37(H37), C38(H38), C39(H39), C41(H41), C42(H42), C43(H43), C44(H44), C45(H45)
2.b Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C7(H7A,H7B,H7C), C8(H8A,
 H8B,H8C), C9(H9A,H9B,H9C)
;
_shelx_res_checksum              83316
_olex2_submission_special_instructions
;
   1  0.000  0.000  0.000       513    146 
;
_platon_squeeze_void_probe_radius 1.20