#------------------------------------------------------------------------------
#$Date: 2020-09-02 19:55:10 +0300 (Wed, 02 Sep 2020) $
#$Revision: 255805 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/31/97/4319766.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_4319766
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 Ga I2 N2'
_chemical_formula_weight         741.11
_chemical_melting_point          225
_chemical_name_common            NacNacGaI2
_chemical_name_systematic
; 

 ? 

;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 113.3880(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.8237(7)
_cell_length_b                   8.6190(3)
_cell_length_c                   20.0720(7)
_cell_measurement_reflns_used    7980
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      31.4
_cell_measurement_theta_min      2.35
_cell_volume                     2988.95(19)
_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 0.949
_diffrn_measured_fraction_theta_max 0.949
_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  0.0219
_diffrn_reflns_av_sigmaI/netI    0.0179
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            38669
_diffrn_reflns_theta_full        31.47
_diffrn_reflns_theta_max         31.47
_diffrn_reflns_theta_min         1.91
_diffrn_standards_decay_%        <0.01
_diffrn_standards_number         '50 frames remeasured'
_exptl_absorpt_coefficient_mu    3.759
_exptl_absorpt_correction_T_max  0.5202
_exptl_absorpt_correction_T_min  0.2113
_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    2.103
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelipiped
_exptl_crystal_F_000             1880
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.546
_refine_diff_density_min         -0.835
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.659
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         9427
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.659
_refine_ls_R_factor_all          0.0216
_refine_ls_R_factor_gt           0.0185
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0475P)²+5.7346P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0504
_refine_ls_wR_factor_ref         0.0528
_reflns_number_gt                8634
_reflns_number_total             9427
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic001311d_7.cif
_cod_data_source_block           nh10
_cod_depositor_comments
;

2020-09-02
Z value changed to be consistent with given formula
                 miguel
;
_cod_original_formula_units_Z            5
_cod_original_cell_volume        2988.95(18)
_cod_database_code               4319766
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
I1 I 0.822540(6) 0.192567(12) 0.121210(5) 0.01876(3) Uani 1 1 d . . .
I2 I 1.058023(6) 0.256493(11) 0.186129(5) 0.01655(3) Uani 1 1 d . . .
Ga3 Ga 0.956494(9) 0.097870(18) 0.206111(8) 0.01104(3) Uani 1 1 d . . .
N2 N 0.95795(7) 0.09533(14) 0.30366(7) 0.0123(2) Uani 1 1 d . . .
N1 N 0.97063(7) -0.12014(14) 0.19475(7) 0.0119(2) Uani 1 1 d . . .
C6 C 1.00781(8) -0.18191(16) 0.14954(8) 0.0128(2) Uani 1 1 d . . .
C11 C 0.96420(9) -0.21383(18) 0.07586(8) 0.0162(3) Uani 1 1 d . . .
C18 C 0.97775(8) 0.23349(16) 0.34820(8) 0.0128(2) Uani 1 1 d . . .
C3 C 0.93677(8) -0.03615(17) 0.32604(8) 0.0131(2) Uani 1 1 d . . .
C7 C 1.08775(9) -0.21497(17) 0.18251(8) 0.0150(3) Uani 1 1 d . . .
C12 C 0.87877(9) -0.17647(18) 0.03871(9) 0.0188(3) Uani 1 1 d . . .
H12A H 0.8610 -0.1362 0.0762 0.023 Uiso 1 1 calc R . .
C2 C 0.92410(9) -0.17695(17) 0.28823(8) 0.0149(3) Uani 1 1 d . . .
H2A H 0.8974 -0.2538 0.3033 0.018 Uiso 1 1 calc R . .
C1 C 0.94524(8) -0.22045(17) 0.23139(8) 0.0132(2) Uani 1 1 d . . .
C9 C 1.07994(11) -0.3178(2) 0.06739(10) 0.0243(3) Uani 1 1 d . . .
H9A H 1.1045 -0.3653 0.0394 0.029 Uiso 1 1 calc R . .
C5 C 0.92537(9) -0.04052(18) 0.39646(8) 0.0181(3) Uani 1 1 d . . .
H5A H 0.9501 0.0504 0.4258 0.027 Uiso 1 1 calc R . .
H5B H 0.9487 -0.1352 0.4232 0.027 Uiso 1 1 calc R . .
H5C H 0.8699 -0.0396 0.3860 0.027 Uiso 1 1 calc R . .
C10 C 1.00211(11) -0.2827(2) 0.03588(9) 0.0217(3) Uani 1 1 d . . .
H10A H 0.9736 -0.3057 -0.0140 0.026 Uiso 1 1 calc R . .
C13 C 0.86525(12) -0.0495(2) -0.01854(10) 0.0280(4) Uani 1 1 d . . .
H13A H 0.8957 0.0425 0.0044 0.042 Uiso 1 1 calc R . .
H13B H 0.8102 -0.0224 -0.0401 0.042 Uiso 1 1 calc R . .
H13C H 0.8813 -0.0875 -0.0565 0.042 Uiso 1 1 calc R . .
C15 C 1.13574(9) -0.18374(19) 0.26224(9) 0.0191(3) Uani 1 1 d . . .
H15A H 1.1055 -0.1125 0.2804 0.023 Uiso 1 1 calc R . .
C24 C 1.11937(8) 0.15690(19) 0.38638(8) 0.0170(3) Uani 1 1 d . . .
H24A H 1.1001 0.1007 0.3389 0.020 Uiso 1 1 calc R . .
C23 C 1.05700(8) 0.27072(18) 0.38443(8) 0.0146(3) Uani 1 1 d . . .
C17 C 1.21280(10) -0.1042(2) 0.27435(12) 0.0296(4) Uani 1 1 d . . .
H17A H 1.2028 -0.0100 0.2446 0.044 Uiso 1 1 calc R . .
H17B H 1.2453 -0.1751 0.2604 0.044 Uiso 1 1 calc R . .
H17C H 1.2395 -0.0765 0.3257 0.044 Uiso 1 1 calc R . .
C8 C 1.12227(10) -0.2837(2) 0.13996(10) 0.0211(3) Uani 1 1 d . . .
H8A H 1.1759 -0.3076 0.1611 0.025 Uiso 1 1 calc R . .
C4 C 0.93903(9) -0.39017(17) 0.21209(9) 0.0181(3) Uani 1 1 d . . .
H4A H 0.9816 -0.4193 0.1983 0.027 Uiso 1 1 calc R . .
H4B H 0.8895 -0.4098 0.1713 0.027 Uiso 1 1 calc R . .
H4C H 0.9419 -0.4518 0.2541 0.027 Uiso 1 1 calc R . .
C26 C 1.19621(10) 0.2338(2) 0.39652(10) 0.0245(3) Uani 1 1 d . . .
H26A H 1.1872 0.3126 0.3588 0.037 Uiso 1 1 calc R . .
H26B H 1.2320 0.1552 0.3928 0.037 Uiso 1 1 calc R . .
H26C H 1.2186 0.2829 0.4444 0.037 Uiso 1 1 calc R . .
C16 C 1.15089(11) -0.3342(2) 0.30681(10) 0.0285(4) Uani 1 1 d . . .
H16A H 1.1015 -0.3787 0.3030 0.043 Uiso 1 1 calc R . .
H16B H 1.1830 -0.3114 0.3578 0.043 Uiso 1 1 calc R . .
H16C H 1.1778 -0.4086 0.2881 0.043 Uiso 1 1 calc R . .
C14 C 0.83042(12) -0.3207(2) 0.00371(12) 0.0320(4) Uani 1 1 d . . .
H14A H 0.8420 -0.4036 0.0399 0.048 Uiso 1 1 calc R . .
H14B H 0.8431 -0.3558 -0.0367 0.048 Uiso 1 1 calc R . .
H14C H 0.7753 -0.2948 -0.0144 0.048 Uiso 1 1 calc R . .
C19 C 0.91972(9) 0.33041(17) 0.35324(8) 0.0145(2) Uani 1 1 d . . .
C27 C 0.83346(9) 0.29405(19) 0.31938(9) 0.0176(3) Uani 1 1 d . . .
H27A H 0.8259 0.1949 0.2915 0.021 Uiso 1 1 calc R . .
C20 C 0.94318(9) 0.46810(18) 0.39343(8) 0.0178(3) Uani 1 1 d . . .
H20A H 0.9051 0.5344 0.3981 0.021 Uiso 1 1 calc R . .
C29 C 0.78737(9) 0.4219(2) 0.26702(10) 0.0214(3) Uani 1 1 d . . .
H29A H 0.8075 0.4362 0.2292 0.032 Uiso 1 1 calc R . .
H29B H 0.7925 0.5192 0.2938 0.032 Uiso 1 1 calc R . .
H29C H 0.7327 0.3922 0.2445 0.032 Uiso 1 1 calc R . .
C21 C 1.02033(10) 0.50954(19) 0.42639(9) 0.0204(3) Uani 1 1 d . . .
H21A H 1.0347 0.6053 0.4517 0.024 Uiso 1 1 calc R . .
C22 C 1.07669(9) 0.41036(19) 0.42230(9) 0.0188(3) Uani 1 1 d . . .
H22A H 1.1297 0.4384 0.4458 0.023 Uiso 1 1 calc R . .
C28 C 0.80057(11) 0.2730(2) 0.37812(11) 0.0253(3) Uani 1 1 d . . .
H28A H 0.8327 0.1988 0.4147 0.038 Uiso 1 1 calc R . .
H28B H 0.7474 0.2336 0.3556 0.038 Uiso 1 1 calc R . .
H28C H 0.8007 0.3730 0.4013 0.038 Uiso 1 1 calc R . .
C25 C 1.13275(10) 0.0360(2) 0.44652(11) 0.0272(4) Uani 1 1 d . . .
H25A H 1.0836 -0.0147 0.4392 0.041 Uiso 1 1 calc R . .
H25B H 1.1533 0.0875 0.4939 0.041 Uiso 1 1 calc R . .
H25C H 1.1699 -0.0420 0.4448 0.041 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'
Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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'
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 Ga3 N2 99.25(5) . . ?
N1 Ga3 I2 111.31(4) . . ?
N2 Ga3 I2 117.35(4) . . ?
N1 Ga3 I1 112.31(4) . . ?
N2 Ga3 I1 106.90(4) . . ?
I2 Ga3 I1 109.413(7) . . ?
C3 N2 C18 121.89(12) . . ?
C3 N2 Ga3 117.41(10) . . ?
C18 N2 Ga3 120.64(9) . . ?
C1 N1 C6 118.21(12) . . ?
C1 N1 Ga3 117.95(10) . . ?
C6 N1 Ga3 123.84(9) . . ?
C11 C6 C7 121.51(13) . . ?
C11 C6 N1 120.37(13) . . ?
C7 C6 N1 118.06(13) . . ?
C10 C11 C6 117.96(15) . . ?
C10 C11 C12 119.42(14) . . ?
C6 C11 C12 122.63(13) . . ?
C19 C18 C23 121.21(13) . . ?
C19 C18 N2 121.01(13) . . ?
C23 C18 N2 117.74(12) . . ?
N2 C3 C2 124.17(13) . . ?
N2 C3 C5 120.47(13) . . ?
C2 C3 C5 115.36(13) . . ?
C8 C7 C6 117.90(14) . . ?
C8 C7 C15 119.64(14) . . ?
C6 C7 C15 122.43(13) . . ?
C11 C12 C14 111.93(14) . . ?
C11 C12 C13 110.40(14) . . ?
C14 C12 C13 110.06(15) . . ?
C1 C2 C3 129.14(13) . . ?
N1 C1 C2 123.58(13) . . ?
N1 C1 C4 119.58(13) . . ?
C2 C1 C4 116.84(13) . . ?
C10 C9 C8 119.88(15) . . ?
C9 C10 C11 121.36(16) . . ?
C7 C15 C17 112.09(14) . . ?
C7 C15 C16 111.07(14) . . ?
C17 C15 C16 109.87(14) . . ?
C23 C24 C26 113.83(14) . . ?
C23 C24 C25 110.00(13) . . ?
C26 C24 C25 109.74(14) . . ?
C22 C23 C18 118.36(14) . . ?
C22 C23 C24 120.57(14) . . ?
C18 C23 C24 120.94(13) . . ?
C9 C8 C7 121.38(15) . . ?
C20 C19 C18 117.77(14) . . ?
C20 C19 C27 117.82(13) . . ?
C18 C19 C27 124.39(13) . . ?
C19 C27 C29 111.78(13) . . ?
C19 C27 C28 111.28(14) . . ?
C29 C27 C28 108.58(13) . . ?
C21 C20 C19 121.63(14) . . ?
C20 C21 C22 119.62(15) . . ?
C23 C22 C21 121.30(15) . . ?
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
I1 Ga3 2.5528(2) . ?
I2 Ga3 2.50820(19) . ?
Ga3 N1 1.9240(12) . ?
Ga3 N2 1.9475(12) . ?
N2 C3 1.3369(18) . ?
N2 C18 1.4462(18) . ?
N1 C1 1.3401(18) . ?
N1 C6 1.4494(18) . ?
C6 C11 1.405(2) . ?
C6 C7 1.412(2) . ?
C11 C10 1.400(2) . ?
C11 C12 1.515(2) . ?
C18 C19 1.410(2) . ?
C18 C23 1.413(2) . ?
C3 C2 1.401(2) . ?
C3 C5 1.512(2) . ?
C7 C8 1.394(2) . ?
C7 C15 1.517(2) . ?
C12 C14 1.536(2) . ?
C12 C13 1.533(2) . ?
C2 C1 1.400(2) . ?
C1 C4 1.506(2) . ?
C9 C10 1.379(3) . ?
C9 C8 1.386(3) . ?
C15 C17 1.534(2) . ?
C15 C16 1.537(3) . ?
C24 C23 1.519(2) . ?
C24 C26 1.529(2) . ?
C24 C25 1.538(2) . ?
C23 C22 1.393(2) . ?
C19 C20 1.404(2) . ?
C19 C27 1.523(2) . ?
C27 C29 1.533(2) . ?
C27 C28 1.545(2) . ?
C20 C21 1.383(2) . ?
C21 C22 1.390(2) . ?
