#------------------------------------------------------------------------------
#$Date: 2016-03-23 21:43:14 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179455 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/52/4335294.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_4335294
loop_
_publ_author_name
'Erandi Bernabé-Pablo'
'Vojtech Jancik'
'Mónica Moya-Cabrera'
_publ_section_title
;
 A Synthetic Route to a Molecular Galloxane Dihydroxide and Its Group 4
 Heterobimetallic Compounds
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6944
_journal_page_last               6950
_journal_paper_doi               10.1021/ic4010054
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C46 H58 Cl2 Ga2 N4 O'
_chemical_formula_sum            'C46 H58 Cl2 Ga2 N4 O'
_chemical_formula_weight         893.30
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           43
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.539(3)
_cell_length_b                   47.199(5)
_cell_length_c                   9.343(2)
_cell_measurement_reflns_used    6858
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      2.16
_cell_volume                     9057(3)
_computing_cell_refinement       'Bruker AXS SAINT (v 7.34A, Bruker 2006)'
_computing_data_collection       'SMART V 5.625 (Bruker, 1999)'
_computing_data_reduction        'Bruker AXS SAINT (v 7.34A, Bruker 2006)'
_computing_molecular_graphics    'Bruker AXS SHELXTL (v 6.12)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 0.661
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker Smart Apex CCD diffractometer'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0294
_diffrn_reflns_av_sigmaI/netI    0.0485
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       56
_diffrn_reflns_limit_k_min       -52
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            9363
_diffrn_reflns_theta_full        25.04
_diffrn_reflns_theta_max         25.04
_diffrn_reflns_theta_min         1.73
_exptl_absorpt_coefficient_mu    1.345
_exptl_absorpt_correction_T_max  0.741
_exptl_absorpt_correction_T_min  0.617
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs, Sheldrick 2008'
_exptl_crystal_colour            COLORLESS
_exptl_crystal_density_diffrn    1.310
_exptl_crystal_description       PRISM
_exptl_crystal_F_000             3728
_exptl_crystal_size_max          0.372
_exptl_crystal_size_mid          0.344
_exptl_crystal_size_min          0.226
_refine_diff_density_max         0.363
_refine_diff_density_min         -0.292
_refine_diff_density_rms         0.056
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.006(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     257
_refine_ls_number_reflns         3594
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0268
_refine_ls_R_factor_gt           0.0252
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0178P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0548
_refine_ls_wR_factor_ref         0.0553
_reflns_number_gt                3441
_reflns_number_total             3594
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4010054_si_001_2.cif
_cod_data_source_block           Compound3
_cod_database_code               4335294
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'x+1/4, -y+1/4, z+1/4'
'-x+1/4, y+1/4, z+1/4'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'x+1/4, -y+3/4, z+3/4'
'-x+1/4, y+3/4, z+3/4'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'x+3/4, -y+1/4, z+3/4'
'-x+3/4, y+1/4, z+3/4'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'x+3/4, -y+3/4, z+1/4'
'-x+3/4, y+3/4, z+1/4'
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
Ga1 Ga 0.326343(12) 0.253167(5) 0.71582(3) 0.01575(8) Uani 1 1 d .
Cl1 Cl 0.32680(3) 0.229979(14) 0.51197(6) 0.02200(15) Uani 1 1 d .
O1 O 0.2500 0.2500 0.8052(3) 0.0183(5) Uani 1 2 d S
N1 N 0.35516(9) 0.29179(4) 0.6892(2) 0.0176(5) Uani 1 1 d .
N2 N 0.39894(10) 0.23993(5) 0.8276(2) 0.0185(5) Uani 1 1 d .
C1 C 0.43728(13) 0.32948(6) 0.6864(3) 0.0275(7) Uani 1 1 d .
H1A H 0.4238 0.3350 0.5897 0.041 Uiso 1 1 calc R
H1B H 0.4848 0.3309 0.6943 0.041 Uiso 1 1 calc R
H1C H 0.4169 0.3421 0.7564 0.041 Uiso 1 1 calc R
C2 C 0.41639(11) 0.29942(5) 0.7153(3) 0.0198(5) Uani 1 1 d .
C3 C 0.46321(12) 0.28109(6) 0.7727(3) 0.0211(6) Uani 1 1 d .
H3A H 0.5068 0.2878 0.7697 0.025 Uiso 1 1 calc R
C4 C 0.45465(13) 0.25451(6) 0.8335(3) 0.0210(6) Uani 1 1 d .
C5 C 0.51101(13) 0.24189(6) 0.9134(3) 0.0310(7) Uani 1 1 d .
H5A H 0.5208 0.2231 0.8744 0.046 Uiso 1 1 calc R
H5B H 0.4998 0.2402 1.0150 0.046 Uiso 1 1 calc R
H5C H 0.5492 0.2542 0.9029 0.046 Uiso 1 1 calc R
C6 C 0.30826(12) 0.31367(5) 0.6551(3) 0.0182(5) Uani 1 1 d .
C7 C 0.29645(13) 0.32104(5) 0.5113(3) 0.0208(6) Uani 1 1 d .
C8 C 0.25289(11) 0.34278(5) 0.4844(3) 0.0231(6) Uani 1 1 d .
H8A H 0.2451 0.3481 0.3879 0.028 Uiso 1 1 calc R
C9 C 0.22013(13) 0.35713(6) 0.5922(3) 0.0262(6) Uani 1 1 d .
C10 C 0.23193(12) 0.34863(5) 0.7326(3) 0.0255(6) Uani 1 1 d .
H10A H 0.2093 0.3579 0.8078 0.031 Uiso 1 1 calc R
C11 C 0.27532(12) 0.32722(5) 0.7671(3) 0.0210(6) Uani 1 1 d .
C12 C 0.28630(14) 0.31855(6) 0.9198(3) 0.0260(7) Uani 1 1 d .
H12A H 0.2613 0.3310 0.9833 0.039 Uiso 1 1 calc R
H12B H 0.3327 0.3201 0.9427 0.039 Uiso 1 1 calc R
H12C H 0.2721 0.2989 0.9331 0.039 Uiso 1 1 calc R
C13 C 0.32861(13) 0.30535(6) 0.3899(3) 0.0238(6) Uani 1 1 d .
H13A H 0.3197 0.3152 0.2996 0.036 Uiso 1 1 calc R
H13B H 0.3113 0.2860 0.3849 0.036 Uiso 1 1 calc R
H13C H 0.3757 0.3046 0.4061 0.036 Uiso 1 1 calc R
C14 C 0.17393(16) 0.38104(7) 0.5617(4) 0.0387(8) Uani 1 1 d .
H14A H 0.1672 0.3826 0.4581 0.058 Uiso 1 1 calc R
H14B H 0.1923 0.3988 0.5981 0.058 Uiso 1 1 calc R
H14C H 0.1322 0.3773 0.6088 0.058 Uiso 1 1 calc R
C15 C 0.39267(12) 0.21466(5) 0.9143(3) 0.0181(5) Uani 1 1 d .
C16 C 0.41087(13) 0.18824(6) 0.8614(3) 0.0234(6) Uani 1 1 d .
C17 C 0.40661(12) 0.16495(6) 0.9529(3) 0.0255(6) Uani 1 1 d .
H17A H 0.4195 0.1469 0.9185 0.031 Uiso 1 1 calc R
C18 C 0.38413(13) 0.16736(6) 1.0919(3) 0.0245(6) Uani 1 1 d .
C19 C 0.36525(13) 0.19413(6) 1.1403(3) 0.0226(6) Uani 1 1 d .
H19A H 0.3495 0.1960 1.2354 0.027 Uiso 1 1 calc R
C20 C 0.36880(12) 0.21786(6) 1.0546(3) 0.0199(6) Uani 1 1 d .
C21 C 0.34916(15) 0.24639(6) 1.1100(3) 0.0273(6) Uani 1 1 d .
H21A H 0.3334 0.2445 1.2086 0.041 Uiso 1 1 calc R
H21B H 0.3144 0.2541 1.0498 0.041 Uiso 1 1 calc R
H21C H 0.3868 0.2591 1.1080 0.041 Uiso 1 1 calc R
C22 C 0.43574(14) 0.18437(6) 0.7098(3) 0.0314(7) Uani 1 1 d .
H22A H 0.4513 0.1649 0.6973 0.047 Uiso 1 1 calc R
H22B H 0.4716 0.1976 0.6922 0.047 Uiso 1 1 calc R
H22C H 0.4004 0.1881 0.6419 0.047 Uiso 1 1 calc R
C23 C 0.38049(15) 0.14194(6) 1.1891(3) 0.0338(7) Uani 1 1 d .
H23A H 0.3921 0.1476 1.2868 0.051 Uiso 1 1 calc R
H23B H 0.4109 0.1274 1.1555 0.051 Uiso 1 1 calc R
H23C H 0.3361 0.1343 1.1882 0.051 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'
O O 0.0106 0.0060 '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
O1 Ga1 N2 113.57(9) .
O1 Ga1 N1 114.12(6) .
N2 Ga1 N1 97.97(9) .
O1 Ga1 Cl1 111.60(6) .
N2 Ga1 Cl1 107.79(7) .
N1 Ga1 Cl1 110.93(6) .
Ga1 O1 Ga1 124.15(14) 14
C2 N1 C6 118.4(2) .
C2 N1 Ga1 121.40(16) .
C6 N1 Ga1 119.83(15) .
C4 N2 C15 118.5(2) .
C4 N2 Ga1 121.22(18) .
C15 N2 Ga1 120.14(16) .
N1 C2 C3 123.5(2) .
N1 C2 C1 119.4(2) .
C3 C2 C1 117.0(2) .
C4 C3 C2 128.9(2) .
N2 C4 C3 123.9(2) .
N2 C4 C5 118.5(2) .
C3 C4 C5 117.7(2) .
C11 C6 C7 121.1(2) .
C11 C6 N1 118.8(2) .
C7 C6 N1 120.0(2) .
C8 C7 C6 117.9(2) .
C8 C7 C13 120.7(2) .
C6 C7 C13 121.4(2) .
C7 C8 C9 122.9(3) .
C8 C9 C10 117.3(2) .
C8 C9 C14 122.4(3) .
C10 C9 C14 120.4(3) .
C11 C10 C9 122.8(3) .
C10 C11 C6 118.0(3) .
C10 C11 C12 121.1(2) .
C6 C11 C12 120.9(2) .
C16 C15 C20 121.3(2) .
C16 C15 N2 121.1(2) .
C20 C15 N2 117.6(2) .
C15 C16 C17 118.2(2) .
C15 C16 C22 122.0(2) .
C17 C16 C22 119.9(2) .
C18 C17 C16 122.1(2) .
C17 C18 C19 118.1(2) .
C17 C18 C23 121.2(2) .
C19 C18 C23 120.7(2) .
C20 C19 C18 122.1(2) .
C19 C20 C15 118.2(2) .
C19 C20 C21 121.0(2) .
C15 C20 C21 120.8(2) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ga1 O1 1.7827(12) .
Ga1 N2 1.925(2) .
Ga1 N1 1.933(2) .
Ga1 Cl1 2.1967(7) .
O1 Ga1 1.7826(11) 14
N1 C2 1.331(3) .
N1 C6 1.448(3) .
N2 C4 1.336(3) .
N2 C15 1.447(3) .
C1 C2 1.507(4) .
C2 C3 1.400(4) .
C3 C4 1.388(4) .
C4 C5 1.501(4) .
C6 C11 1.400(4) .
C6 C7 1.409(4) .
C7 C8 1.385(4) .
C7 C13 1.507(4) .
C8 C9 1.387(4) .
C9 C10 1.393(4) .
C9 C14 1.502(4) .
C10 C11 1.385(4) .
C11 C12 1.501(4) .
C15 C16 1.393(4) .
C15 C20 1.408(4) .
C16 C17 1.395(4) .
C16 C22 1.517(4) .
C17 C18 1.383(4) .
C18 C19 1.397(4) .
C18 C23 1.507(4) .
C19 C20 1.379(4) .
C20 C21 1.498(4) .
