Structurally characterised intermediate of the oxidative addition of a heteroleptic germylene to gallanediyle
Bücker, Anna; Wölper, Christoph; Haberhauer, Gebhard; Schulz, Stephan; Chemical Communications  (2022) –; doi:10.1039/D2CC03561H

data_7130494
_publ_section_title
;
 Structurally characterised intermediate of the oxidative addition of a
 heteroleptic germylene to gallanediyle
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC03561H
_journal_year                    2022
_chemical_formula_sum            'C47.5 H71 Cl Ga Ge N3 Si'
_chemical_formula_weight         889.92
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2022-03-18 deposited with the CCDC.	2022-08-05 downloaded from the CCDC.
;
_cell_angle_alpha                81.3746(13)
_cell_angle_beta                 85.1409(14)
_cell_angle_gamma                67.7274(13)
_cell_formula_units_Z            2
_cell_length_a                   10.2306(5)
_cell_length_b                   12.1923(6)
_cell_length_c                   20.7888(10)
_cell_measurement_reflns_used    9663
_cell_measurement_temperature    102(2)
_cell_measurement_theta_max      80.66
_cell_measurement_theta_min      4.67
_cell_volume                     2371.4(2)
_computing_cell_refinement       'Bruker APEX3(v2017.3-0)'
_computing_data_collection       'Bruker APEX3(v2017.3-0)'
_computing_data_reduction        'Bruker APEX3(v2017.3-0)'
_computing_molecular_graphics    'ORTEP/PLATON (Spek)'
_computing_publication_material  'BRUKER AXS SHELXTL (c) 2008 / Vers. 2008/4'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'Bruker APEX3(v2017.3-0)'
_diffrn_ambient_temperature      102(2)
_diffrn_detector_area_resol_mean 7.3910
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker D8 Venture (Photon II detector)'
_diffrn_measurement_method       'Data collection strategy APEX 3/Queen'
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0285
_diffrn_reflns_av_unetI/netI     0.0116
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            136125
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         80.765
_diffrn_reflns_theta_min         2.150
_diffrn_source                   'micro-focus sealed tube'
_diffrn_source_type              'INCOATEC I\mS 3.0'
_exptl_absorpt_coefficient_mu    2.482
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.63
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 SADABS
 R.H. Blessing, Acta Cryst. (1995) A51 33-38 
;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.246
_exptl_crystal_description       tablet
_exptl_crystal_F_000             942
_exptl_crystal_size_max          0.192
_exptl_crystal_size_mid          0.103
_exptl_crystal_size_min          0.092
_refine_diff_density_max         0.606
_refine_diff_density_min         -0.525
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     529
_refine_ls_number_reflns         10317
_refine_ls_number_restraints     130
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0244
_refine_ls_R_factor_gt           0.0239
_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^)+(0.0300P)^2^+1.4667P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0628
_refine_ls_wR_factor_ref         0.0632
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10038
_reflns_number_total             10317
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc03561h2.cif
_cod_data_source_block           ab_191m
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_atom_sites_solution_secondary' value 'diffmap' was
changed to 'difmap'.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_formula_sum        'C47.50 H71 Cl Ga Ge N3 Si'
_cod_database_code               7130494
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.647
_shelx_estimated_absorpt_t_max   0.804
_shelx_res_checksum              14423
_shelx_hkl_checksum              69247