Acyclic α-Phosphinoamido-Germylene: Synthesis and Characterization
Pal, Shiv; Dasgupta, Rajarshi; Khan, Shabana; Organometallics 35 (2016) 3635–; doi:10.1021/acs.organomet.6b00689

data_4089073
_publ_section_title
;
 Acyclic \a-Phosphinoamido-Germylene: Synthesis and Characterization
;
_journal_issue                   20
_journal_name_full               Organometallics
_journal_page_first              3635
_journal_paper_doi               10.1021/acs.organomet.6b00689
_journal_volume                  35
_journal_year                    2016
_chemical_formula_sum            'C48 H54 Ge N2 P2'
_chemical_formula_weight         793.46
_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_method           SHELXL-2014/6
_cell_angle_alpha                95.526(5)
_cell_angle_beta                 91.930(6)
_cell_angle_gamma                90.621(5)
_cell_formula_units_Z            4
_cell_length_a                   10.754(2)
_cell_length_b                   17.660(3)
_cell_length_c                   22.507(4)
_cell_measurement_reflns_used    7683
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      22.20
_cell_measurement_theta_min      2.35
_cell_volume                     4251.7(13)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.1910
_diffrn_reflns_av_unetI/netI     0.1438
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            80912
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.248
_diffrn_reflns_theta_min         2.249
_exptl_absorpt_coefficient_mu    0.830
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Sheldrick,G.M(2012)SADABS.BrukerAXS Inc.,Madison,Wisconsin,USA.'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.239
_exptl_crystal_description       block
_exptl_crystal_F_000             1672
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   0.7457
_exptl_transmission_factor_min   0.6200
_refine_diff_density_max         1.367
_refine_diff_density_min         -0.780
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     971
_refine_ls_number_reflns         15370
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.1447
_refine_ls_R_factor_gt           0.0644
_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^)+(0.0615P)^2^+2.0486P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1276
_refine_ls_wR_factor_ref         0.1577
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8612
_reflns_number_total             15370
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00689_si_002.cif
_cod_data_source_block           3
_cod_original_cell_volume        4252.0(14)
_cod_database_code               4089073
_shelxl_version_number           2014/6
_shelx_res_checksum              76006
_shelx_hkl_checksum              2025