The Reactivity of Germanium Phosphanides with Chalcogens
Harris, Lisa M.; Tam, Eric C. Y.; Cummins, Struan J. W.; Coles, Martyn P.; Fulton, J. Robin; Inorganic Chemistry  (2017) –; doi:10.1021/acs.inorgchem.6b03109

data_4345235
_publ_section_title
;
 The Reactivity of Germanium Phosphanides with Chalcogens
;
_journal_name_full               'Inorganic Chemistry'
_journal_paper_doi               10.1021/acs.inorgchem.6b03109
_journal_year                    2017
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         '2(C41 H51 Ge1 N2 P1 Se2), C4 H10 O'
_chemical_formula_sum            'C86 H112 Ge2 N4 O P2 Se4'
_chemical_formula_weight         1740.76
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2011-07-08T08:42:36-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                81.251(2)
_cell_angle_beta                 78.847(2)
_cell_angle_gamma                66.679(2)
_cell_formula_units_Z            1
_cell_length_a                   10.8309(4)
_cell_length_b                   12.7855(4)
_cell_length_c                   16.7183(7)
_cell_measurement_reflns_used    17587
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.733
_cell_measurement_theta_min      3.395
_cell_measurement_wavelength     0.71073
_cell_volume                     2078.49(14)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Bruker AXS Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.84086E-2
_diffrn_orient_matrix_UB_12      -0.197514E-1
_diffrn_orient_matrix_UB_13      0.594388E-1
_diffrn_orient_matrix_UB_21      0.965609E-1
_diffrn_orient_matrix_UB_22      -0.59929E-2
_diffrn_orient_matrix_UB_23      -0.120943E-1
_diffrn_orient_matrix_UB_31      -0.306039E-1
_diffrn_orient_matrix_UB_32      0.82943E-1
_diffrn_orient_matrix_UB_33      0.79951E-2
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0665
_diffrn_reflns_av_unetI/netI     0.0744
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            26100
_diffrn_reflns_theta_full        26.73
_diffrn_reflns_theta_max         26.73
_diffrn_reflns_theta_min         3.46
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    2.559
_exptl_absorpt_correction_T_max  0.8615
_exptl_absorpt_correction_T_min  0.756
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.391
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Rhombohedral
_exptl_crystal_F_000             894
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.717
_refine_diff_density_min         -0.776
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     471
_refine_ls_number_reflns         8776
_refine_ls_number_restraints     33
_refine_ls_restrained_S_all      0.991
_refine_ls_R_factor_all          0.0788
_refine_ls_R_factor_gt           0.0448
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0194P)^2^+2.9822P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0763
_refine_ls_wR_factor_ref         0.0857
_reflns_number_gt                6333
_reflns_number_total             8776
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b03109_si_002.cif
_cod_data_source_block           Compound-4PhSe
_cod_original_cell_volume        2078.49(13)
_cod_database_code               4345235