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_7130496
_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            'C60 H67 Al F36 Ga N3 O4 Si Sn'
_chemical_formula_weight         1821.64
_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'
_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                90
_cell_angle_beta                 113.542(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.3750(16)
_cell_length_b                   19.8369(15)
_cell_length_c                   20.6724(17)
_cell_measurement_reflns_used    9747
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      79.25
_cell_measurement_theta_min      3.17
_cell_volume                     8035.8(11)
_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      100(2)
_diffrn_detector_area_resol_mean 7.3910
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_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  0.0871
_diffrn_reflns_av_unetI/netI     0.0408
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            228480
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         79.850
_diffrn_reflns_theta_min         2.255
_diffrn_source                   'micro-focus sealed tube'
_diffrn_source_type              'INCOATEC I\mS 3.0'
_exptl_absorpt_coefficient_mu    4.285
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.44
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 SADABS
 R.H. Blessing, Acta Cryst. (1995) A51 33-38 
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.506
_exptl_crystal_description       block
_exptl_crystal_F_000             3648
_exptl_crystal_size_max          0.439
_exptl_crystal_size_mid          0.404
_exptl_crystal_size_min          0.385
_refine_diff_density_max         1.823
_refine_diff_density_min         -0.760
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1436
_refine_ls_number_reflns         17440
_refine_ls_number_restraints     9844
_refine_ls_restrained_S_all      0.907
_refine_ls_R_factor_all          0.0563
_refine_ls_R_factor_gt           0.0502
_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^)+(0.0900P)^2^+5.2621P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1355
_refine_ls_wR_factor_ref         0.1436
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15333
_reflns_number_total             17440
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc03561h2.cif
_cod_data_source_block           ab_047bm_sq
_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_sg_symbol_H-M      'P 21/c'
_cod_database_code               7130496
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.255
_shelx_estimated_absorpt_t_max   0.289
_shelx_res_checksum              89237
_shelx_hkl_checksum              86335
_shelx_fab_checksum              21633