C4-Ferrocenylsilyl-bridged and -substituted N-heterocyclic carbenes: complexation of germanium chloride.
Wang, Yuzhong; Hickox, Hunter P.; Wei, Pingrong; Robinson, Gregory H.; Dalton transactions (Cambridge, England : 2003) 46 (2017) 5508–5512; doi:10.1039/c7dt00066a

data_7042869
_publ_section_title
;
 C4-Ferrocenylsilyl-bridged and -substituted N-heterocyclic carbenes:
 complexation of germanium chloride.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5508
_journal_page_last               5512
_journal_paper_doi               10.1039/c7dt00066a
_journal_volume                  46
_journal_year                    2017
_chemical_formula_sum            'C76 H106 Cl4 Fe Ge2 N4 O2 Si2'
_chemical_formula_weight         1506.65
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-01-02 deposited with the CCDC.
2017-02-17 downloaded from the CCDC.
;
_cell_angle_alpha                80.614(2)
_cell_angle_beta                 82.073(2)
_cell_angle_gamma                82.496(2)
_cell_formula_units_Z            2
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_cell_length_b                   16.9634(12)
_cell_length_c                   20.1520(14)
_cell_measurement_reflns_used    9777
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      23.93
_cell_measurement_theta_min      2.24
_cell_volume                     4047.3(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker D8 Quest PHOTON 100 CMOS'
_diffrn_measurement_method       'Phi\Omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0532
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            16757
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.519
_diffrn_reflns_theta_min         2.421
_diffrn_source                   Imus
_exptl_absorpt_coefficient_mu    1.120
_exptl_absorpt_correction_T_max  0.745372
_exptl_absorpt_correction_T_min  0.533245
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'BRUKER TWINABS'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.236
_exptl_crystal_description       plate
_exptl_crystal_F_000             1584
_exptl_crystal_size_max          0.320
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_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.568
_refine_diff_density_min         -0.559
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     916
_refine_ls_number_reflns         16757
_refine_ls_number_restraints     392
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.1155
_refine_ls_R_factor_gt           0.0653
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0992P)^2^+1.8101P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1599
_refine_ls_wR_factor_ref         0.1898
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10889
_reflns_number_total             16757
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00066a2.cif
_cod_data_source_block           twin5
_cod_database_code               7042869
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.716
_shelx_estimated_absorpt_t_max   0.850
_shelx_res_checksum              98372