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#$Date: 2022-03-01 01:48:56 +0200 (Tue, 01 Mar 2022) $
#$Revision: 273183 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/96/7709615.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_7709615
loop_
_publ_author_name
'Roesky, Herbert W.'
'Kumar, Arun'
'Banerjee, Samya'
'Sharma, Nishant'
'Nazish, Mohd'
'Graw, Nico'
'Herbst-Irmer, Regine'
'Lourderaj, Upakarasamy'
'Stalke, Dietmar'
_publ_section_title
;
 Synthesis and computational aspects of Al(II)-Al(II) and Ga(II)-Ga(II)
 dihalides based on an amidinate scaffold
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00317A
_journal_year                    2022
_chemical_formula_moiety         'C30 H46 Cl2 Ga2 N4'
_chemical_formula_sum            'C30 H46 Cl2 Ga2 N4'
_chemical_formula_weight         673.05
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-01-25 deposited with the CCDC.	2022-02-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 114.36(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.069(3)
_cell_length_b                   8.896(2)
_cell_length_c                   17.634(2)
_cell_measurement_reflns_used    2979
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.274
_cell_measurement_theta_min      2.4765
_cell_volume                     3296.7(11)
_computing_cell_refinement       'SAINT V8.38A'
_computing_data_collection       'APEX2 v2012.2'
_computing_data_reduction        'SAINT V8.38A'
_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 0.996
_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  0.0776
_diffrn_reflns_av_unetI/netI     0.0187
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            146235
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.475
_diffrn_reflns_theta_min         1.938
_diffrn_source                   'INCOATEC Microsource'
_exptl_absorpt_coefficient_mu    1.821
_exptl_absorpt_correction_T_max  0.745372
_exptl_absorpt_correction_T_min  0.521630
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   TWINABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.356
_exptl_crystal_description       block
_exptl_crystal_F_000             1400
_exptl_crystal_size_max          0.376
_exptl_crystal_size_mid          0.171
_exptl_crystal_size_min          0.163
_refine_diff_density_max         0.505
_refine_diff_density_min         -0.350
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     178
_refine_ls_number_reflns         3406
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0409
_refine_ls_R_factor_gt           0.0337
_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/[σ²(Fo²)+(0.0338P)²+7.9639P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0768
_refine_ls_wR_factor_ref         0.0797
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3093
_reflns_number_total             3406
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2dt00317a2.cif
_cod_data_source_block           twin4
_cod_original_cell_volume        3296.7(10)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7709615
_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   0.548
_shelx_estimated_absorpt_t_max   0.756
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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 0.44306(2) 0.74260(3) 0.22604(2) 0.01747(9) Uani 1 1 d . . . . .
Cl1 Cl 0.38987(3) 0.88502(7) 0.11632(4) 0.02462(14) Uani 1 1 d . . . . .
N1 N 0.40031(9) 0.7363(2) 0.30303(12) 0.0167(4) Uani 1 1 d . . . . .
N2 N 0.39555(9) 0.5534(2) 0.21729(12) 0.0187(4) Uani 1 1 d . . . . .
C1 C 0.37938(10) 0.5961(3) 0.27826(14) 0.0171(5) Uani 1 1 d . . . . .
C2 C 0.34290(11) 0.5037(3) 0.31429(14) 0.0183(5) Uani 1 1 d . . . . .
C3 C 0.37391(12) 0.3964(3) 0.37529(15) 0.0223(5) Uani 1 1 d . . . . .
H3 H 0.418181 0.379178 0.392615 0.027 Uiso 1 1 calc R U . . .
C4 C 0.34015(13) 0.3150(3) 0.41066(16) 0.0265(6) Uani 1 1 d . . . . .
H4 H 0.361285 0.242028 0.452310 0.032 Uiso 1 1 calc R U . . .
C5 C 0.27570(13) 0.3399(3) 0.38528(16) 0.0274(6) Uani 1 1 d . . . . .
H5 H 0.252652 0.284320 0.409740 0.033 Uiso 1 1 calc R U . . .
C6 C 0.24457(12) 0.4457(3) 0.32433(16) 0.0257(5) Uani 1 1 d . . . . .
H6 H 0.200234 0.462001 0.306900 0.031 Uiso 1 1 calc R U . . .
C7 C 0.27806(11) 0.5277(3) 0.28872(15) 0.0206(5) Uani 1 1 d . . . . .
H7 H 0.256698 0.600254 0.246928 0.025 Uiso 1 1 calc R U . . .
C8 C 0.41264(11) 0.8108(3) 0.38346(14) 0.0187(5) Uani 1 1 d . . . . .
C9 C 0.46829(12) 0.7330(3) 0.45325(15) 0.0231(5) Uani 1 1 d . . . . .
H9A H 0.478134 0.786194 0.505811 0.035 Uiso 1 1 calc R U . . .
H9B H 0.505658 0.734375 0.440185 0.035 Uiso 1 1 calc R U . . .
H9C H 0.456741 0.628772 0.458503 0.035 Uiso 1 1 calc R U . . .
C10 C 0.35411(12) 0.8158(3) 0.40352(16) 0.0246(5) Uani 1 1 d . . . . .
H10A H 0.362581 0.882383 0.451210 0.037 Uiso 1 1 calc R U . . .
H10B H 0.344734 0.714395 0.417051 0.037 Uiso 1 1 calc R U . . .
H10C H 0.317552 0.853933 0.355147 0.037 Uiso 1 1 calc R U . . .
C11 C 0.43158(13) 0.9717(3) 0.37362(16) 0.0257(5) Uani 1 1 d . . . . .
H11A H 0.441225 1.027353 0.425391 0.039 Uiso 1 1 calc R U . . .
H11B H 0.396389 1.020909 0.327914 0.039 Uiso 1 1 calc R U . . .
H11C H 0.469268 0.970112 0.361243 0.039 Uiso 1 1 calc R U . . .
C12 C 0.37328(13) 0.4267(3) 0.15835(16) 0.0247(5) Uani 1 1 d . . . . .
C13 C 0.30583(14) 0.4583(4) 0.09349(18) 0.0374(7) Uani 1 1 d . . . . .
H13A H 0.276871 0.466621 0.121218 0.056 Uiso 1 1 calc R U . . .
H13B H 0.291921 0.375811 0.053078 0.056 Uiso 1 1 calc R U . . .
H13C H 0.305484 0.552631 0.064612 0.056 Uiso 1 1 calc R U . . .
C14 C 0.3762(2) 0.2763(3) 0.2006(2) 0.0451(8) Uani 1 1 d . . . . .
H14A H 0.343610 0.273212 0.222708 0.068 Uiso 1 1 calc R U . . .
H14B H 0.418348 0.263615 0.246322 0.068 Uiso 1 1 calc R U . . .
H14C H 0.368622 0.195067 0.160090 0.068 Uiso 1 1 calc R U . . .
C15 C 0.41882(14) 0.4226(3) 0.11537(18) 0.0327(6) Uani 1 1 d . . . . .
H15A H 0.462223 0.404236 0.156863 0.049 Uiso 1 1 calc R U . . .
H15B H 0.417279 0.519116 0.087795 0.049 Uiso 1 1 calc R U . . .
H15C H 0.406145 0.341846 0.073887 0.049 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
N2 Ga1 N1 67.26(8) . . ?
N2 Ga1 Cl1 109.22(6) . . ?
N1 Ga1 Cl1 111.23(6) . . ?
N2 Ga1 Ga1 121.11(6) . 2_655 ?
N1 Ga1 Ga1 122.66(6) . 2_655 ?
Cl1 Ga1 Ga1 116.01(3) . 2_655 ?
N2 Ga1 C1 33.46(8) . . ?
N1 Ga1 C1 33.85(7) . . ?
Cl1 Ga1 C1 115.96(6) . . ?
Ga1 Ga1 C1 127.93(5) 2_655 . ?
C1 N1 C8 128.81(19) . . ?
C1 N1 Ga1 90.98(14) . . ?
C8 N1 Ga1 133.63(15) . . ?
C1 N2 C12 131.0(2) . . ?
C1 N2 Ga1 91.43(14) . . ?
C12 N2 Ga1 136.52(15) . . ?
N2 C1 N1 110.2(2) . . ?
N2 C1 C2 125.6(2) . . ?
N1 C1 C2 124.3(2) . . ?
N2 C1 Ga1 55.11(12) . . ?
N1 C1 Ga1 55.17(11) . . ?
C2 C1 Ga1 177.17(17) . . ?
C7 C2 C3 119.8(2) . . ?
C7 C2 C1 119.8(2) . . ?
C3 C2 C1 120.4(2) . . ?
C4 C3 C2 120.0(2) . . ?
C5 C4 C3 119.9(2) . . ?
C4 C5 C6 120.3(2) . . ?
C5 C6 C7 120.1(2) . . ?
C6 C7 C2 119.9(2) . . ?
N1 C8 C11 105.12(18) . . ?
N1 C8 C9 109.53(19) . . ?
C11 C8 C9 109.3(2) . . ?
N1 C8 C10 113.3(2) . . ?
C11 C8 C10 108.6(2) . . ?
C9 C8 C10 110.8(2) . . ?
N2 C12 C14 113.3(2) . . ?
N2 C12 C15 104.9(2) . . ?
C14 C12 C15 108.7(2) . . ?
N2 C12 C13 109.8(2) . . ?
C14 C12 C13 110.7(2) . . ?
C15 C12 C13 109.2(2) . . ?
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 N2 1.9795(19) . ?
Ga1 N1 1.9807(19) . ?
Ga1 Cl1 2.2126(8) . ?
Ga1 Ga1 2.4053(6) 2_655 ?
Ga1 C1 2.413(2) . ?
N1 C1 1.344(3) . ?
N1 C8 1.482(3) . ?
N2 C1 1.331(3) . ?
N2 C12 1.474(3) . ?
C1 C2 1.493(3) . ?
C2 C7 1.389(3) . ?
C2 C3 1.394(3) . ?
C3 C4 1.386(3) . ?
C4 C5 1.383(4) . ?
C5 C6 1.385(4) . ?
C6 C7 1.387(3) . ?
C8 C11 1.528(3) . ?
C8 C9 1.529(3) . ?
C8 C10 1.531(3) . ?
C12 C14 1.520(4) . ?
C12 C15 1.528(3) . ?
C12 C13 1.530(4) . ?
