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

data_4089074
_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 Ge2 N2 O P2'
_chemical_formula_weight         882.05
_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-2014/7
_cell_angle_alpha                105.161(12)
_cell_angle_beta                 94.562(13)
_cell_angle_gamma                105.937(13)
_cell_formula_units_Z            2
_cell_length_a                   9.348(5)
_cell_length_b                   12.975(6)
_cell_length_c                   19.947(9)
_cell_measurement_reflns_used    9651
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      23.66
_cell_measurement_theta_min      2.31
_cell_volume                     2215.4(19)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_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  0.0899
_diffrn_reflns_av_unetI/netI     0.0457
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            85853
_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         25.246
_diffrn_reflns_theta_min         2.270
_exptl_absorpt_coefficient_mu    1.466
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Sheldrick, G.M.(2012) SADABS.Bruker AXS Inc.,Madison,Wisconsin, USA.'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.322
_exptl_crystal_description       block
_exptl_crystal_F_000             916
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   0.1524
_exptl_transmission_factor_min   0.1063
_refine_diff_density_max         0.573
_refine_diff_density_min         -0.536
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     504
_refine_ls_number_reflns         8026
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0629
_refine_ls_R_factor_gt           0.0414
_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^)+(0.0273P)^2^+2.4682P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0878
_refine_ls_wR_factor_ref         0.0957
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6263
_reflns_number_total             8026
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00689_si_002.cif
_cod_data_source_block           4
_cod_original_cell_volume        2215.5(18)
_cod_database_code               4089074
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              434
_shelx_hkl_checksum              94529