#------------------------------------------------------------------------------
#$Date: 2016-03-23 04:07:30 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179277 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/97/4319761.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_4319761
loop_
_publ_author_name
'Matthias Stender'
'Barrett E. Eichler'
'Ned J. Hardman'
'Philip P. Power'
'Jörg Prust'
'Mathias Noltemeyer'
'Herbert W. Roesky'
_publ_section_title
;
 Synthesis and Characterization of HC{C(Me)N(C6H3-2,6-i-Pr2)}2MX2 (M = Al,
 X = Cl, I; M = Ga, In, X = Me, Cl, I): Sterically Encumbered
 β-Diketiminate Group 13 Metal Derivatives
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2794
_journal_page_last               2799
_journal_paper_doi               10.1021/ic001311d
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C29 H41 Cl2 Ga N2'
_chemical_formula_weight         558.26
_chemical_name_common            NacNacGaCl2
_chemical_name_systematic
; 

 ? 

;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 108.432(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.0709(13)
_cell_length_b                   13.0948(10)
_cell_length_c                   13.7356(10)
_cell_measurement_reflns_used    3521
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      27.75
_cell_measurement_theta_min      2.21
_cell_volume                     2912.9(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL v. 5.10'
_computing_molecular_graphics    'XP, Bruker SHELXTL v. 5.10'
_computing_publication_material  'XCIF, Bruker SHELXTL v. 5.10'
_computing_structure_refinement  'XL, Bruker SHELXTL v. 5.10'
_computing_structure_solution    'XS, Bruker SHELXTL v. 5.10'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method       /w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0414
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            40038
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         2.00
_diffrn_standards_decay_%        <0.01
_diffrn_standards_number         '50 frames remeasured'
_exptl_absorpt_coefficient_mu    1.147
_exptl_absorpt_correction_T_max  0.8467
_exptl_absorpt_correction_T_min  0.7947
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;SADABS: an empirical absorption program by G. M. Sheldrick

using the method described by Blessing, R. H.; Acta Cryst.

A51, 1995, 33.

;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.273
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1176
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.788
_refine_diff_density_min         -0.430
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         3804
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0564
_refine_ls_R_factor_gt           0.0400
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0617P)²+3.8617P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1025
_refine_ls_wR_factor_ref         0.1118
_reflns_number_gt                3010
_reflns_number_total             3804
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic001311d_2.cif
_cod_data_source_block           be43a
_cod_database_code               4319761
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ga1 Ga 0.28918(3) 0.88527(3) 1.02645(3) 0.01777(17) Uani 1 1 d . . .
Cl1 Cl 0.21291(6) 0.79986(8) 1.10411(8) 0.0199(3) Uani 1 1 d . . .
Cl2 Cl 0.38024(6) 0.98322(8) 1.13855(8) 0.0230(3) Uani 1 1 d . . .
N1 N 0.3478(2) 0.7988(3) 0.9595(3) 0.0184(8) Uani 1 1 d . . .
N2 N 0.2248(2) 0.9639(2) 0.9124(3) 0.0184(8) Uani 1 1 d . . .
C1 C 0.3563(2) 0.8304(3) 0.8708(3) 0.0197(10) Uani 1 1 d . . .
C2 C 0.3182(2) 0.9186(3) 0.8190(3) 0.0198(10) Uani 1 1 d . . .
H2A H 0.3393 0.9422 0.7667 0.024 Uiso 1 1 calc R . .
C3 C 0.2545(2) 0.9764(3) 0.8328(3) 0.0192(10) Uani 1 1 d . . .
C4 C 0.4077(3) 0.7697(3) 0.8210(3) 0.0244(10) Uani 1 1 d . . .
H4A H 0.4223 0.7040 0.8563 0.037 Uiso 1 1 calc R . .
H4B H 0.4582 0.8076 0.8254 0.037 Uiso 1 1 calc R . .
H4C H 0.3762 0.7578 0.7488 0.037 Uiso 1 1 calc R . .
C5 C 0.2156(3) 1.0584(3) 0.7543(3) 0.0243(10) Uani 1 1 d . . .
H5A H 0.2177 1.1241 0.7892 0.036 Uiso 1 1 calc R . .
H5B H 0.1580 1.0405 0.7181 0.036 Uiso 1 1 calc R . .
H5C H 0.2461 1.0636 0.7048 0.036 Uiso 1 1 calc R . .
C6 C 0.3871(3) 0.7054(3) 1.0103(3) 0.0193(10) Uani 1 1 d . . .
C7 C 0.3390(3) 0.6157(3) 1.0007(3) 0.0219(10) Uani 1 1 d . . .
C8 C 0.3779(3) 0.5285(3) 1.0516(3) 0.0265(11) Uani 1 1 d . . .
H8A H 0.3468 0.4674 1.0463 0.032 Uiso 1 1 calc R . .
C9 C 0.4598(3) 0.5281(3) 1.1091(3) 0.0271(11) Uani 1 1 d . . .
H9A H 0.4847 0.4674 1.1428 0.033 Uiso 1 1 calc R . .
C10 C 0.5061(3) 0.6163(3) 1.1180(3) 0.0240(10) Uani 1 1 d . . .
H10A H 0.5629 0.6150 1.1577 0.029 Uiso 1 1 calc R . .
C11 C 0.4718(3) 0.7076(3) 1.0700(3) 0.0207(10) Uani 1 1 d . . .
C12 C 0.5259(2) 0.8013(3) 1.0848(3) 0.0232(10) Uani 1 1 d . . .
H12A H 0.4917 0.8592 1.0462 0.028 Uiso 1 1 calc R . .
C13 C 0.5992(3) 0.7855(4) 1.0442(4) 0.0339(12) Uani 1 1 d . . .
H13A H 0.5787 0.7639 0.9722 0.051 Uiso 1 1 calc R . .
H13B H 0.6359 0.7328 1.0850 0.051 Uiso 1 1 calc R . .
H13C H 0.6298 0.8497 1.0494 0.051 Uiso 1 1 calc R . .
C14 C 0.5586(3) 0.8307(4) 1.1994(3) 0.0277(11) Uani 1 1 d . . .
H14A H 0.5119 0.8403 1.2256 0.042 Uiso 1 1 calc R . .
H14B H 0.5902 0.8944 1.2073 0.042 Uiso 1 1 calc R . .
H14C H 0.5943 0.7762 1.2381 0.042 Uiso 1 1 calc R . .
C15 C 0.2497(3) 0.6084(3) 0.9324(3) 0.0273(11) Uani 1 1 d . . .
H15A H 0.2291 0.6791 0.9117 0.033 Uiso 1 1 calc R . .
C16 C 0.1937(3) 0.5593(4) 0.9872(4) 0.0352(12) Uani 1 1 d . . .
H16A H 0.1983 0.5972 1.0502 0.053 Uiso 1 1 calc R . .
H16B H 0.2106 0.4883 1.0043 0.053 Uiso 1 1 calc R . .
H16C H 0.1363 0.5609 0.9420 0.053 Uiso 1 1 calc R . .
C17 C 0.2449(3) 0.5488(4) 0.8359(4) 0.0395(13) Uani 1 1 d . . .
H17A H 0.2802 0.5816 0.8008 0.059 Uiso 1 1 calc R . .
H17B H 0.1877 0.5478 0.7902 0.059 Uiso 1 1 calc R . .
H17C H 0.2639 0.4787 0.8543 0.059 Uiso 1 1 calc R . .
C18 C 0.1427(2) 1.0016(3) 0.9046(3) 0.0178(10) Uani 1 1 d . . .
C19 C 0.1337(2) 1.0900(3) 0.9579(3) 0.0201(10) Uani 1 1 d . . .
C20 C 0.0538(3) 1.1209(3) 0.9504(3) 0.0245(11) Uani 1 1 d . . .
H20A H 0.0464 1.1800 0.9867 0.029 Uiso 1 1 calc R . .
C21 C -0.0146(3) 1.0680(3) 0.8916(3) 0.0236(10) Uani 1 1 d . . .
H21A H -0.0686 1.0907 0.8870 0.028 Uiso 1 1 calc R . .
C22 C -0.0040(3) 0.9816(3) 0.8394(3) 0.0239(10) Uani 1 1 d . . .
H22A H -0.0512 0.9458 0.7982 0.029 Uiso 1 1 calc R . .
C23 C 0.0743(3) 0.9456(3) 0.8456(3) 0.0221(10) Uani 1 1 d . . .
C24 C 0.0809(3) 0.8476(3) 0.7881(4) 0.0277(11) Uani 1 1 d . . .
H24A H 0.1410 0.8323 0.8029 0.033 Uiso 1 1 calc R . .
C25 C 0.0424(3) 0.7576(4) 0.8264(4) 0.0373(12) Uani 1 1 d . . .
H25A H 0.0677 0.7511 0.9009 0.056 Uiso 1 1 calc R . .
H25B H 0.0519 0.6949 0.7930 0.056 Uiso 1 1 calc R . .
H25C H -0.0171 0.7690 0.8101 0.056 Uiso 1 1 calc R . .
C26 C 0.0430(3) 0.8610(4) 0.6711(4) 0.0397(13) Uani 1 1 d . . .
H26A H 0.0560 0.8012 0.6362 0.060 Uiso 1 1 calc R . .
H26B H 0.0659 0.9224 0.6495 0.060 Uiso 1 1 calc R . .
H26C H -0.0171 0.8680 0.6533 0.060 Uiso 1 1 calc R . .
C27 C 0.2067(3) 1.1532(3) 1.0219(3) 0.0250(11) Uani 1 1 d . . .
H27A H 0.2583 1.1218 1.0156 0.030 Uiso 1 1 calc R . .
C28 C 0.2022(3) 1.2635(4) 0.9836(4) 0.0359(12) Uani 1 1 d . . .
H28A H 0.1978 1.2637 0.9107 0.054 Uiso 1 1 calc R . .
H28B H 0.2523 1.3001 1.0229 0.054 Uiso 1 1 calc R . .
H28C H 0.1538 1.2972 0.9927 0.054 Uiso 1 1 calc R . .
C29 C 0.2120(3) 1.1506(4) 1.1356(3) 0.0324(12) Uani 1 1 d . . .
H29A H 0.2126 1.0796 1.1581 0.049 Uiso 1 1 calc R . .
H29B H 0.1640 1.1858 1.1445 0.049 Uiso 1 1 calc R . .
H29C H 0.2627 1.1849 1.1767 0.049 Uiso 1 1 calc R . .
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 100.19(14) . . ?
N2 Ga1 Cl2 110.69(11) . . ?
N1 Ga1 Cl2 108.39(10) . . ?
N2 Ga1 Cl1 113.12(10) . . ?
N1 Ga1 Cl1 113.82(11) . . ?
Cl2 Ga1 Cl1 110.20(4) . . ?
C1 N1 C6 121.9(3) . . ?
C1 N1 Ga1 118.3(3) . . ?
C6 N1 Ga1 119.6(3) . . ?
C3 N2 C18 119.8(3) . . ?
C3 N2 Ga1 117.6(3) . . ?
C18 N2 Ga1 122.3(3) . . ?
N1 C1 C2 123.4(4) . . ?
N1 C1 C4 119.9(4) . . ?
C2 C1 C4 116.6(4) . . ?
C3 C2 C1 129.6(4) . . ?
N2 C3 C2 123.7(4) . . ?
N2 C3 C5 118.0(4) . . ?
C2 C3 C5 118.4(4) . . ?
C11 C6 C7 121.7(4) . . ?
C11 C6 N1 119.3(4) . . ?
C7 C6 N1 119.0(4) . . ?
C8 C7 C6 117.6(4) . . ?
C8 C7 C15 118.9(4) . . ?
C6 C7 C15 123.3(4) . . ?
C9 C8 C7 122.0(4) . . ?
C8 C9 C10 119.9(4) . . ?
C9 C10 C11 121.9(4) . . ?
C10 C11 C6 116.9(4) . . ?
C10 C11 C12 118.9(4) . . ?
C6 C11 C12 124.2(4) . . ?
C11 C12 C13 112.0(4) . . ?
C11 C12 C14 110.4(4) . . ?
C13 C12 C14 109.3(3) . . ?
C17 C15 C7 109.7(4) . . ?
C17 C15 C16 110.1(4) . . ?
C7 C15 C16 112.5(4) . . ?
C19 C18 C23 121.7(4) . . ?
C19 C18 N2 120.1(4) . . ?
C23 C18 N2 118.1(4) . . ?
C20 C19 C18 117.8(4) . . ?
C20 C19 C27 119.1(4) . . ?
C18 C19 C27 123.1(4) . . ?
C21 C20 C19 121.7(4) . . ?
C20 C21 C22 119.3(4) . . ?
C21 C22 C23 121.8(4) . . ?
C22 C23 C18 117.7(4) . . ?
C22 C23 C24 118.5(4) . . ?
C18 C23 C24 123.7(4) . . ?
C25 C24 C23 111.1(4) . . ?
C25 C24 C26 111.4(4) . . ?
C23 C24 C26 111.6(4) . . ?
C19 C27 C28 111.8(4) . . ?
C19 C27 C29 110.5(4) . . ?
C28 C27 C29 110.5(4) . . ?
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 1.906(3) . ?
Ga1 N1 1.926(3) . ?
Ga1 Cl2 2.2179(11) . ?
Ga1 Cl1 2.2276(11) . ?
N1 C1 1.337(5) . ?
N1 C6 1.461(5) . ?
N2 C3 1.353(5) . ?
N2 C18 1.458(5) . ?
C1 C2 1.403(6) . ?
C1 C4 1.501(6) . ?
C2 C3 1.387(6) . ?
C3 C5 1.518(6) . ?
C6 C11 1.419(6) . ?
C6 C7 1.415(6) . ?
C7 C8 1.393(6) . ?
C7 C15 1.520(6) . ?
C8 C9 1.371(6) . ?
C9 C10 1.383(6) . ?
C10 C11 1.401(6) . ?
C11 C12 1.511(6) . ?
C12 C13 1.537(6) . ?
C12 C14 1.543(6) . ?
C15 C17 1.518(6) . ?
C15 C16 1.532(7) . ?
C18 C19 1.403(6) . ?
C18 C23 1.400(6) . ?
C19 C20 1.396(6) . ?
C19 C27 1.522(6) . ?
C20 C21 1.379(6) . ?
C21 C22 1.382(6) . ?
C22 C23 1.395(6) . ?
C23 C24 1.529(6) . ?
C24 C25 1.522(7) . ?
C24 C26 1.541(7) . ?
C27 C28 1.530(6) . ?
C27 C29 1.536(6) . ?
