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_4345236
_publ_section_title
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 The Reactivity of Germanium Phosphanides with Chalcogens
;
_journal_name_full               'Inorganic Chemistry'
_journal_paper_doi               10.1021/acs.inorgchem.6b03109
_journal_year                    2017
_chemical_formula_moiety         'C41 H63 Ge N2 P S3, C7 H8'
_chemical_formula_sum            'C48 H71 Ge N2 P S3'
_chemical_formula_weight         875.80
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-12-02
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.30 svn.r3368 for OlexSys, GUI svn.r5269)
;
_cell_angle_alpha                90
_cell_angle_beta                 101.1518(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.37898(13)
_cell_length_b                   21.0070(3)
_cell_length_c                   22.1248(4)
_cell_measurement_reflns_used    47091
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      71.7190
_cell_measurement_theta_min      4.4210
_cell_volume                     4732.81(13)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
;
_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 (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0856
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.9991
_diffrn_measured_fraction_theta_max 0.9972
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0472548000
_diffrn_orient_matrix_UB_12      0.0117018000
_diffrn_orient_matrix_UB_13      -0.0694962000
_diffrn_orient_matrix_UB_21      0.0014560000
_diffrn_orient_matrix_UB_22      0.0723296000
_diffrn_orient_matrix_UB_23      0.0115996000
_diffrn_orient_matrix_UB_31      0.1437109000
_diffrn_orient_matrix_UB_32      0.0031009000
_diffrn_orient_matrix_UB_33      -0.0085190000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0279
_diffrn_reflns_av_unetI/netI     0.0146
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            67482
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.863
_diffrn_reflns_theta_min         4.586
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.678
_exptl_absorpt_correction_T_max  0.434
_exptl_absorpt_correction_T_min  0.236
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.229
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rhombohedral
_exptl_crystal_F_000             1872
_exptl_crystal_size_max          0.4278
_exptl_crystal_size_mid          0.3151
_exptl_crystal_size_min          0.2413
_refine_diff_density_max         0.574
_refine_diff_density_min         -0.446
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     507
_refine_ls_number_reflns         9268
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0288
_refine_ls_R_factor_gt           0.0282
_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^)+(0.0330P)^2^+3.0700P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0704
_refine_ls_wR_factor_ref         0.0708
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9104
_reflns_number_total             9268
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b03109_si_002.cif
_cod_data_source_block           Compound-5CyS
_cod_original_cell_volume        4732.80(13)
_cod_database_code               4345236
_chemical_oxdiff_formula         'C48 H71 Ge N2 P S3'
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C24(H24), C30(H30), C15(H15), C12(H12), C36(H36), C27(H27)
2.b Secondary CH2 refined with riding coordinates:
 C33(H33A,H33B), C35(H35A,H35B), C31(H31A,H31B), C34(H34A,H34B), C32(H32A,
 H32B), C39(H39A,H39B), C37(H37A,H37B), C41(H41A,H41B), C40(H40A,H40B),
 C38(H38A,H38B)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C21(H21), C10(H10), C8(H8), C20(H20), C22(H22), C9(H9), C43(H43),
 C44(H44), C47(H47), C45(H45), C46(H46)
2.d Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C14(H14A,H14B,H14C), C4(H4A,H4B,
 H4C), C13(H13A,H13B,H13C), C17(H17A,H17B,H17C), C28(H28A,H28B,H28C), C5(H5A,
 H5B,H5C), C29(H29A,H29B,H29C), C16(H16A,H16B,H16C), C48(H48A,H48B,H48C)
;