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#$Date: 2021-07-05 20:28:56 +0300 (Mon, 05 Jul 2021) $
#$Revision: 267144 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/75/7707503.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_7707503
loop_
_publ_author_name
'Dehmel, Maximilian'
'Köhler, Angelina'
'Görls, Helmar'
'Kretschmer, Robert'
_publ_section_title
;
 Synthesis, characterization, and reactivity of group 13 hydride complexes
 based on amido-amine ligands.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8434
_journal_page_last               8445
_journal_paper_doi               10.1039/d1dt01454d
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C38 H62 Cl2 Ga2 N4'
_chemical_formula_sum            'C38 H62 Cl2 Ga2 N4'
_chemical_formula_weight         785.25
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-04-21 deposited with the CCDC.	2021-05-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.529(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.9859(3)
_cell_length_b                   12.6693(6)
_cell_length_c                   17.0024(7)
_cell_measurement_reflns_used    14269
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      27.472
_cell_measurement_theta_min      2.407
_cell_volume                     1926.63(14)
_computing_cell_refinement       DENZO
_computing_data_collection       COLLECT
_computing_data_reduction        DENZO
_computing_molecular_graphics    SHELXTL/PC
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'phi + omega - scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0456
_diffrn_reflns_av_unetI/netI     0.0359
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            14269
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.472
_diffrn_reflns_theta_min         2.407
_exptl_absorpt_coefficient_mu    1.569
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6551
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., 
 J. Appl. Cryst. 48 (2015) 3-10 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.354
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             828
_exptl_crystal_size_max          0.092
_exptl_crystal_size_mid          0.088
_exptl_crystal_size_min          0.078
_refine_diff_density_max         0.656
_refine_diff_density_min         -0.382
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.155
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     212
_refine_ls_number_reflns         4405
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.155
_refine_ls_R_factor_all          0.0552
_refine_ls_R_factor_gt           0.0437
_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)+(0.0261P)²+2.8184P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0900
_refine_ls_wR_factor_ref         0.0950
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3789
_reflns_number_total             4405
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1dt01454d2.cif
_cod_data_source_block           FO6933_10a
_cod_depositor_comments
'Adding full bibliography for 7707498--7707509.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7707503
_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   0.869
_shelx_estimated_absorpt_t_max   0.887
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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
Ga1 Ga 0.38126(3) 0.52795(2) 0.46489(2) 0.02107(9) Uani 1 1 d . . . . .
Cl1 Cl 0.21868(8) 0.56221(6) 0.55563(4) 0.02979(17) Uani 1 1 d . . . . .
N1 N 0.3496(3) 0.62357(18) 0.37982(13) 0.0233(5) Uani 1 1 d . . . . .
N2 N 0.2482(2) 0.42434(19) 0.39300(14) 0.0240(5) Uani 1 1 d . . . . .
C1 C 0.2245(3) 0.5952(3) 0.32192(18) 0.0322(7) Uani 1 1 d . . . . .
H1A H 0.262543 0.575944 0.271080 0.039 Uiso 1 1 calc R U . . .
H1B H 0.156129 0.656133 0.312622 0.039 Uiso 1 1 calc R U . . .
C2 C 0.1412(3) 0.5025(2) 0.35334(19) 0.0301(7) Uani 1 1 d . . . . .
H2A H 0.073029 0.528188 0.391539 0.036 Uiso 1 1 calc R U . . .
H2B H 0.080040 0.467741 0.309182 0.036 Uiso 1 1 calc R U . . .
C3 C 0.3321(4) 0.3713(3) 0.33228(18) 0.0332(7) Uani 1 1 d . . . . .
H3A H 0.391645 0.424706 0.306540 0.040 Uiso 1 1 calc R U . . .
H3B H 0.259951 0.339945 0.291160 0.040 Uiso 1 1 calc R U . . .
C4 C 0.4350(4) 0.2861(3) 0.3677(2) 0.0384(8) Uani 1 1 d . . . . .
H4A H 0.514945 0.318732 0.403873 0.046 Uiso 1 1 calc R U . . .
H4B H 0.482961 0.250238 0.324941 0.046 Uiso 1 1 calc R U . . .
C5 C 0.3530(4) 0.2052(3) 0.4127(2) 0.0422(9) Uani 1 1 d . . . . .
H5A H 0.425842 0.156196 0.440594 0.051 Uiso 1 1 calc R U . . .
H5B H 0.285232 0.163571 0.375219 0.051 Uiso 1 1 calc R U . . .
C6 C 0.2630(4) 0.2595(3) 0.4721(2) 0.0368(8) Uani 1 1 d . . . . .
H6A H 0.201852 0.206370 0.497077 0.044 Uiso 1 1 calc R U . . .
H6B H 0.332076 0.292010 0.514086 0.044 Uiso 1 1 calc R U . . .
C7 C 0.1613(3) 0.3439(2) 0.43318(18) 0.0298(6) Uani 1 1 d . . . . .
H7A H 0.087020 0.310671 0.394029 0.036 Uiso 1 1 calc R U . . .
H7B H 0.106322 0.378866 0.473698 0.036 Uiso 1 1 calc R U . . .
C8 C 0.4120(3) 0.7252(2) 0.37017(16) 0.0250(6) Uani 1 1 d . . . . .
C9 C 0.5455(3) 0.7373(2) 0.33304(17) 0.0275(6) Uani 1 1 d . . . . .
C10 C 0.6048(4) 0.8384(3) 0.32485(18) 0.0350(7) Uani 1 1 d . . . . .
H10A H 0.694181 0.846735 0.299882 0.042 Uiso 1 1 calc R U . . .
C11 C 0.5353(4) 0.9264(3) 0.3525(2) 0.0398(8) Uani 1 1 d . . . . .
H11A H 0.577459 0.994468 0.347117 0.048 Uiso 1 1 calc R U . . .
C12 C 0.4047(4) 0.9149(3) 0.3879(2) 0.0390(8) Uani 1 1 d . . . . .
H12A H 0.357603 0.975753 0.406698 0.047 Uiso 1 1 calc R U . . .
C13 C 0.3398(3) 0.8161(2) 0.39685(17) 0.0298(6) Uani 1 1 d . . . . .
C14 C 0.6238(3) 0.6426(3) 0.30135(18) 0.0321(7) Uani 1 1 d . . . . .
H14A H 0.593869 0.578640 0.330460 0.038 Uiso 1 1 calc R U . . .
C15 C 0.5748(4) 0.6266(4) 0.2136(2) 0.0536(11) Uani 1 1 d . . . . .
H15A H 0.466151 0.617002 0.206114 0.080 Uiso 1 1 calc R U . . .
H15B H 0.624157 0.563879 0.194572 0.080 Uiso 1 1 calc R U . . .
H15C H 0.602693 0.688618 0.183872 0.080 Uiso 1 1 calc R U . . .
C16 C 0.7948(4) 0.6502(3) 0.3115(2) 0.0437(8) Uani 1 1 d . . . . .
H16A H 0.828643 0.662486 0.367296 0.066 Uiso 1 1 calc R U . . .
H16B H 0.827228 0.708830 0.279667 0.066 Uiso 1 1 calc R U . . .
H16C H 0.837888 0.584124 0.294104 0.066 Uiso 1 1 calc R U . . .
C17 C 0.1922(4) 0.8103(3) 0.43372(18) 0.0333(7) Uani 1 1 d . . . . .
H17A H 0.162261 0.734431 0.435872 0.040 Uiso 1 1 calc R U . . .
C18 C 0.0680(4) 0.8700(3) 0.3834(2) 0.0430(8) Uani 1 1 d . . . . .
H18A H -0.026885 0.861313 0.406702 0.065 Uiso 1 1 calc R U . . .
H18B H 0.058240 0.841520 0.329571 0.065 Uiso 1 1 calc R U . . .
H18C H 0.093401 0.945128 0.381927 0.065 Uiso 1 1 calc R U . . .
C19 C 0.2050(4) 0.8541(3) 0.5182(2) 0.0470(9) Uani 1 1 d . . . . .
H19A H 0.107830 0.848559 0.539607 0.071 Uiso 1 1 calc R U . . .
H19B H 0.235589 0.928300 0.517619 0.071 Uiso 1 1 calc R U . . .
H19C H 0.279583 0.813376 0.551329 0.071 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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ga Ga 0.2307 1.6083 '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
N1 Ga1 N2 85.38(10) . . ?
N1 Ga1 Cl1 109.84(8) . . ?
N2 Ga1 Cl1 98.54(7) . . ?
N1 Ga1 Ga1 128.28(7) . 3_666 ?
N2 Ga1 Ga1 121.77(7) . 3_666 ?
Cl1 Ga1 Ga1 108.20(3) . 3_666 ?
C8 N1 C1 115.5(2) . . ?
C8 N1 Ga1 129.70(18) . . ?
C1 N1 Ga1 113.98(18) . . ?
C7 N2 C2 108.5(2) . . ?
C7 N2 C3 109.3(2) . . ?
C2 N2 C3 109.3(2) . . ?
C7 N2 Ga1 117.22(18) . . ?
C2 N2 Ga1 98.90(17) . . ?
C3 N2 Ga1 112.82(18) . . ?
N1 C1 C2 109.0(2) . . ?
N1 C1 H1A 109.9 . . ?
C2 C1 H1A 109.9 . . ?
N1 C1 H1B 109.9 . . ?
C2 C1 H1B 109.9 . . ?
H1A C1 H1B 108.3 . . ?
N2 C2 C1 110.7(2) . . ?
N2 C2 H2A 109.5 . . ?
C1 C2 H2A 109.5 . . ?
N2 C2 H2B 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 108.1 . . ?
N2 C3 C4 112.1(3) . . ?
N2 C3 H3A 109.2 . . ?
C4 C3 H3A 109.2 . . ?
N2 C3 H3B 109.2 . . ?
C4 C3 H3B 109.2 . . ?
H3A C3 H3B 107.9 . . ?
C3 C4 C5 112.1(3) . . ?
C3 C4 H4A 109.2 . . ?
C5 C4 H4A 109.2 . . ?
C3 C4 H4B 109.2 . . ?
C5 C4 H4B 109.2 . . ?
H4A C4 H4B 107.9 . . ?
C4 C5 C6 110.3(3) . . ?
C4 C5 H5A 109.6 . . ?
C6 C5 H5A 109.6 . . ?
C4 C5 H5B 109.6 . . ?
C6 C5 H5B 109.6 . . ?
H5A C5 H5B 108.1 . . ?
C7 C6 C5 111.5(3) . . ?
C7 C6 H6A 109.3 . . ?
C5 C6 H6A 109.3 . . ?
C7 C6 H6B 109.3 . . ?
C5 C6 H6B 109.3 . . ?
H6A C6 H6B 108.0 . . ?
N2 C7 C6 111.2(2) . . ?
N2 C7 H7A 109.4 . . ?
C6 C7 H7A 109.4 . . ?
N2 C7 H7B 109.4 . . ?
C6 C7 H7B 109.4 . . ?
H7A C7 H7B 108.0 . . ?
C13 C8 C9 119.2(3) . . ?
C13 C8 N1 120.1(3) . . ?
C9 C8 N1 120.7(3) . . ?
C10 C9 C8 119.3(3) . . ?
C10 C9 C14 119.7(3) . . ?
C8 C9 C14 121.0(3) . . ?
C11 C10 C9 121.1(3) . . ?
C11 C10 H10A 119.5 . . ?
C9 C10 H10A 119.5 . . ?
C12 C11 C10 119.7(3) . . ?
C12 C11 H11A 120.2 . . ?
C10 C11 H11A 120.2 . . ?
C11 C12 C13 121.7(3) . . ?
C11 C12 H12A 119.2 . . ?
C13 C12 H12A 119.2 . . ?
C12 C13 C8 119.0(3) . . ?
C12 C13 C17 118.5(3) . . ?
C8 C13 C17 122.5(3) . . ?
C9 C14 C15 110.6(3) . . ?
C9 C14 C16 113.9(3) . . ?
C15 C14 C16 108.1(3) . . ?
C9 C14 H14A 108.0 . . ?
C15 C14 H14A 108.0 . . ?
C16 C14 H14A 108.0 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C13 C17 C19 112.3(3) . . ?
C13 C17 C18 111.2(3) . . ?
C19 C17 C18 109.1(3) . . ?
C13 C17 H17A 108.0 . . ?
C19 C17 H17A 108.0 . . ?
C18 C17 H17A 108.0 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
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
Ga1 N1 1.887(2) . ?
Ga1 N2 2.089(2) . ?
Ga1 Cl1 2.2665(8) . ?
Ga1 Ga1 2.4474(6) 3_666 ?
N1 C8 1.420(4) . ?
N1 C1 1.466(4) . ?
N2 C7 1.489(4) . ?
N2 C2 1.495(4) . ?
N2 C3 1.495(4) . ?
C1 C2 1.518(4) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.509(5) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C5 1.512(5) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.518(5) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 C7 1.516(4) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C13 1.417(4) . ?
C8 C9 1.417(4) . ?
C9 C10 1.399(4) . ?
C9 C14 1.516(4) . ?
C10 C11 1.381(5) . ?
C10 H10A 0.9500 . ?
C11 C12 1.377(5) . ?
C11 H11A 0.9500 . ?
C12 C13 1.395(4) . ?
C12 H12A 0.9500 . ?
C13 C17 1.522(4) . ?
C14 C15 1.528(5) . ?
C14 C16 1.533(4) . ?
C14 H14A 1.0000 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C19 1.534(5) . ?
C17 C18 1.538(4) . ?
C17 H17A 1.0000 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
