#------------------------------------------------------------------------------
#$Date: 2021-03-05 04:01:04 +0200 (Fri, 05 Mar 2021) $
#$Revision: 262630 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/64/7706439.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7706439
loop_
_publ_author_name
'Ding, Yi'
'Ruth, Paul Niklas'
'Herbst-Irmer, Regine'
'Stalke, Dietmar'
'Yang, Zhi'
'Roesky, Herbert W.'
_publ_section_title
;
 Pentamethyl- and 1,2,4-tri(tert-butyl)cyclopentadienyl containing p-block
 complexes - differences and similarities.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2067
_journal_page_last               2074
_journal_paper_doi               10.1039/d0dt04412a
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C42 H76 Br2 In2'
_chemical_formula_sum            'C42 H76 Br2 In2'
_chemical_formula_weight         970.48
_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
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-12-11 deposited with the CCDC.	2021-01-18 downloaded from the CCDC.
;
_cell_angle_alpha                71.33(2)
_cell_angle_beta                 73.77(2)
_cell_angle_gamma                77.36(3)
_cell_formula_units_Z            1
_cell_length_a                   9.494(2)
_cell_length_b                   10.197(2)
_cell_length_c                   12.616(3)
_cell_measurement_reflns_used    4445
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.381
_cell_measurement_theta_min      2.353
_cell_volume                     1099.7(4)
_computing_cell_refinement       'SAINT V8.40A'
_computing_data_collection       'APEX2 v2012.2'
_computing_data_reduction        'SAINT V8.40A'
_computing_molecular_graphics    'XP Version 5.1'
_computing_publication_material  'XP Version 5.1'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution
'SHELXT(G.M.Sheldrick,Acta Cryst.(2015)A71,3-8)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Smart APEX II Quazar'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0733
_diffrn_reflns_av_unetI/netI     0.0648
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            22845
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.509
_diffrn_reflns_theta_min         1.749
_diffrn_source                   'INCOATEC Microsource'
_exptl_absorpt_coefficient_mu    2.891
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6201
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2016/2
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.465
_exptl_crystal_description       plate
_exptl_crystal_F_000             496
_exptl_crystal_size_max          0.149
_exptl_crystal_size_mid          0.148
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.712
_refine_diff_density_min         -0.525
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         5060
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0497
_refine_ls_R_factor_gt           0.0350
_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/[σ²(Fo²)+(0.0211P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0692
_refine_ls_wR_factor_ref         0.0748
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4017
_reflns_number_total             5060
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0dt04412a2.cif
_cod_data_source_block           7
_cod_depositor_comments
'Adding full bibliography for 7706437--7706443.cif.'
_cod_original_cell_volume        1099.7(5)
_cod_database_code               7706439
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.673
_shelx_estimated_absorpt_t_max   0.869
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
In1 In 0.37067(2) 0.41311(2) 0.15364(2) 0.01720(8) Uani 1 1 d . . . . .
Br1 Br 0.51593(3) 0.63815(3) 0.06113(3) 0.01938(9) Uani 1 1 d . . . . .
C1 C 0.4813(3) 0.2515(3) 0.2867(3) 0.0160(7) Uani 1 1 d . . . . .
C2 C 0.3477(3) 0.2549(3) 0.3837(3) 0.0162(7) Uani 1 1 d . . . . .
C3 C 0.2580(3) 0.1690(3) 0.3783(3) 0.0177(7) Uani 1 1 d . . . . .
H3 H 0.164562 0.153961 0.429431 0.021 Uiso 1 1 calc R U . . .
C4 C 0.3218(3) 0.1046(3) 0.2863(3) 0.0172(7) Uani 1 1 d . . . . .
C5 C 0.4565(3) 0.1515(3) 0.2334(3) 0.0163(7) Uani 1 1 d . . . . .
H5 H 0.524529 0.123191 0.170840 0.020 Uiso 1 1 calc R U . . .
C6 C 0.6458(3) 0.2541(3) 0.2833(3) 0.0185(7) Uani 1 1 d . . . . .
C7 C 0.6764(3) 0.3790(3) 0.3105(3) 0.0222(8) Uani 1 1 d . . . . .
H7A H 0.782684 0.370815 0.305469 0.033 Uiso 1 1 calc R U . . .
H7B H 0.621038 0.381042 0.388283 0.033 Uiso 1 1 calc R U . . .
H7C H 0.645085 0.465472 0.255126 0.033 Uiso 1 1 calc R U . . .
C8 C 0.7421(3) 0.2537(4) 0.1641(3) 0.0222(8) Uani 1 1 d . . . . .
H8A H 0.704869 0.334242 0.106558 0.033 Uiso 1 1 calc R U . . .
H8B H 0.738454 0.167186 0.147361 0.033 Uiso 1 1 calc R U . . .
H8C H 0.844605 0.259444 0.161797 0.033 Uiso 1 1 calc R U . . .
C9 C 0.6941(4) 0.1178(4) 0.3702(3) 0.0264(8) Uani 1 1 d . . . . .
H9A H 0.686799 0.037436 0.346432 0.040 Uiso 1 1 calc R U . . .
H9B H 0.629441 0.114090 0.446458 0.040 Uiso 1 1 calc R U . . .
H9C H 0.796819 0.115144 0.373082 0.040 Uiso 1 1 calc R U . . .
C10 C 0.3017(3) 0.3411(3) 0.4702(3) 0.0184(7) Uani 1 1 d . . . . .
C11 C 0.3928(4) 0.2851(4) 0.5642(3) 0.0243(8) Uani 1 1 d . . . . .
H11A H 0.497306 0.294645 0.528708 0.036 Uiso 1 1 calc R U . . .
H11B H 0.383222 0.186324 0.602447 0.036 Uiso 1 1 calc R U . . .
H11C H 0.355433 0.338962 0.620705 0.036 Uiso 1 1 calc R U . . .
C12 C 0.1392(3) 0.3300(4) 0.5353(3) 0.0263(8) Uani 1 1 d . . . . .
H12A H 0.075607 0.360227 0.480158 0.039 Uiso 1 1 calc R U . . .
H12B H 0.108825 0.389860 0.587344 0.039 Uiso 1 1 calc R U . . .
H12C H 0.129954 0.232749 0.579880 0.039 Uiso 1 1 calc R U . . .
C13 C 0.3090(4) 0.4972(3) 0.4117(3) 0.0240(8) Uani 1 1 d . . . . .
H13A H 0.410024 0.510060 0.367077 0.036 Uiso 1 1 calc R U . . .
H13B H 0.281365 0.548053 0.470166 0.036 Uiso 1 1 calc R U . . .
H13C H 0.240173 0.533121 0.360311 0.036 Uiso 1 1 calc R U . . .
C14 C 0.2492(3) 0.0118(3) 0.2513(3) 0.0209(7) Uani 1 1 d . . . . .
C15 C 0.1212(4) 0.1006(4) 0.1999(3) 0.0339(9) Uani 1 1 d . . . . .
H15A H 0.159098 0.172801 0.130845 0.051 Uiso 1 1 calc R U . . .
H15B H 0.051313 0.145081 0.256107 0.051 Uiso 1 1 calc R U . . .
H15C H 0.070534 0.041254 0.179474 0.051 Uiso 1 1 calc R U . . .
C16 C 0.3571(4) -0.0519(5) 0.1619(4) 0.0493(13) Uani 1 1 d . . . . .
H16A H 0.308356 -0.113268 0.142015 0.074 Uiso 1 1 calc R U . . .
H16B H 0.442772 -0.106491 0.192537 0.074 Uiso 1 1 calc R U . . .
H16C H 0.390317 0.022576 0.093025 0.074 Uiso 1 1 calc R U . . .
C17 C 0.1897(5) -0.1035(4) 0.3564(3) 0.0448(11) Uani 1 1 d . . . . .
H17A H 0.142366 -0.162761 0.332977 0.067 Uiso 1 1 calc R U . . .
H17B H 0.116762 -0.061337 0.412746 0.067 Uiso 1 1 calc R U . . .
H17C H 0.271631 -0.160418 0.390718 0.067 Uiso 1 1 calc R U . . .
C18 C 0.1411(3) 0.4866(3) 0.1480(3) 0.0218(8) Uani 1 1 d . . . . .
H18A H 0.124565 0.471946 0.078719 0.026 Uiso 1 1 calc R U . . .
H18B H 0.079315 0.427682 0.215684 0.026 Uiso 1 1 calc R U . . .
C19 C 0.0858(3) 0.6402(3) 0.1460(3) 0.0186(7) Uani 1 1 d . . . . .
H19A H 0.091316 0.654035 0.218816 0.022 Uiso 1 1 calc R U . . .
H19B H 0.151571 0.699990 0.082350 0.022 Uiso 1 1 calc R U . . .
C20 C -0.0721(3) 0.6853(3) 0.1308(3) 0.0229(8) Uani 1 1 d . . . . .
H20A H -0.137772 0.626234 0.195272 0.027 Uiso 1 1 calc R U . . .
H20B H -0.077700 0.669232 0.058871 0.027 Uiso 1 1 calc R U . . .
C21 C -0.1292(4) 0.8389(3) 0.1263(3) 0.0291(9) Uani 1 1 d . . . . .
H21A H -0.068887 0.898545 0.059649 0.044 Uiso 1 1 calc R U . . .
H21B H -0.122536 0.856284 0.196690 0.044 Uiso 1 1 calc R U . . .
H21C H -0.232681 0.860392 0.119706 0.044 Uiso 1 1 calc R U . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
In In -0.7276 1.3100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C18 In1 C1 132.49(12) . . ?
C18 In1 C5 120.00(11) . . ?
C1 In1 C5 34.92(10) . . ?
C18 In1 Br1 107.17(9) . . ?
C1 In1 Br1 110.23(8) . . ?
C5 In1 Br1 132.81(7) . . ?
C18 In1 Br1 100.78(9) . 2_665 ?
C1 In1 Br1 110.49(8) . 2_665 ?
C5 In1 Br1 84.76(7) . 2_665 ?
Br1 In1 Br1 85.14(2) . 2_665 ?
In1 Br1 In1 94.86(2) . 2_665 ?
C5 C1 C2 103.8(2) . . ?
C5 C1 C6 115.7(3) . . ?
C2 C1 C6 129.0(3) . . ?
C5 C1 In1 84.05(18) . . ?
C2 C1 In1 94.56(19) . . ?
C6 C1 In1 119.4(2) . . ?
C3 C2 C1 106.6(3) . . ?
C3 C2 C10 122.5(3) . . ?
C1 C2 C10 130.7(3) . . ?
C2 C3 C4 112.2(3) . . ?
C5 C4 C3 106.2(3) . . ?
C5 C4 C14 127.6(3) . . ?
C3 C4 C14 126.1(3) . . ?
C4 C5 C1 111.0(3) . . ?
C4 C5 In1 100.3(2) . . ?
C1 C5 In1 61.03(16) . . ?
C7 C6 C8 106.2(2) . . ?
C7 C6 C9 109.8(3) . . ?
C8 C6 C9 108.6(3) . . ?
C7 C6 C1 116.0(3) . . ?
C8 C6 C1 110.1(3) . . ?
C9 C6 C1 106.0(2) . . ?
C2 C10 C13 112.2(3) . . ?
C2 C10 C12 110.0(3) . . ?
C13 C10 C12 106.1(3) . . ?
C2 C10 C11 112.0(3) . . ?
C13 C10 C11 110.9(3) . . ?
C12 C10 C11 105.3(3) . . ?
C16 C14 C4 111.0(3) . . ?
C16 C14 C15 108.3(3) . . ?
C4 C14 C15 108.5(3) . . ?
C16 C14 C17 109.9(3) . . ?
C4 C14 C17 110.0(3) . . ?
C15 C14 C17 109.1(3) . . ?
C19 C18 In1 116.4(2) . . ?
C20 C19 C18 112.4(3) . . ?
C19 C20 C21 113.5(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
In1 C18 2.158(3) . ?
In1 C1 2.257(3) . ?
In1 C5 2.566(3) . ?
In1 Br1 2.7019(9) . ?
In1 Br1 2.7935(8) 2_665 ?
C1 C5 1.477(4) . ?
C1 C2 1.499(4) . ?
C1 C6 1.557(4) . ?
C2 C3 1.378(4) . ?
C2 C10 1.527(4) . ?
C3 C4 1.436(4) . ?
C4 C5 1.376(4) . ?
C4 C14 1.513(4) . ?
C6 C7 1.523(4) . ?
C6 C8 1.526(4) . ?
C6 C9 1.540(4) . ?
C10 C13 1.533(4) . ?
C10 C12 1.541(4) . ?
C10 C11 1.550(4) . ?
C14 C16 1.509(5) . ?
C14 C15 1.517(5) . ?
C14 C17 1.527(5) . ?
C18 C19 1.533(4) . ?
C19 C20 1.516(4) . ?
C20 C21 1.529(5) . ?
