#------------------------------------------------------------------------------
#$Date: 2017-07-11 14:26:40 +0300 (Tue, 11 Jul 2017) $
#$Revision: 198632 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/11/08/7110886.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_7110886
loop_
_publ_author_name
'Luo, Bing'
'Gladfelter, Wayne L.'
_publ_section_title
;
 1,1-Dimethylhydrazidogallane and a gallium hydrazide with two Ga2N2 rings
 bridged by two NNMe2 ligands
;
_journal_issue                   10
_journal_name_full               'Chemical Communications'
_journal_page_first              825
_journal_paper_doi               10.1039/b001010n
_journal_year                    2000
_chemical_compound_source        'Bing Luo'
_chemical_formula_sum            'C4 H18 Ga2 N4'
_chemical_formula_weight         261.66
_chemical_name_common            99255/BL045
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.000(2)
_cell_angle_beta                 95.323(2)
_cell_angle_gamma                90.000(1)
_cell_formula_units_Z            4
_cell_length_a                   6.8583(5)
_cell_length_b                   19.607(2)
_cell_length_c                   8.0977(6)
_cell_measurement_reflns_used    2084
_cell_measurement_temperature    173(2)
_cell_volume                     1084.21(16)
_computing_cell_refinement       'Saint, Bruker'
_computing_data_collection       'Smart, Bruker'
_computing_data_reduction        'Saint, Bruker'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Smart CCD, Siemens'
_diffrn_measurement_method       omega-scans
_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  0.0378
_diffrn_reflns_av_sigmaI/netI    0.0470
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            3964
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.08
_exptl_absorpt_coefficient_mu    4.920
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5773
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Absorption correction was carried out using the program
SADABS, G. Sheldrick (1999).
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.603
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             528
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.385
_refine_diff_density_min         -0.430
_refine_diff_density_rms         0.088
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.07(3)
_refine_ls_extinction_coef       0.0007(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     132
_refine_ls_number_reflns         1718
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0364
_refine_ls_R_factor_gt           0.0294
_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)+(0.0305P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0612
_refine_ls_wR_factor_ref         0.0635
_reflns_number_gt                1554
_reflns_number_total             1718
_reflns_threshold_expression     2sigma(I)
_cod_data_source_file            b001010nsup1.cif
_cod_data_source_block           99255
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'multi-scans' was replaced
with the value 'multi-scan' as specified in the replacement file
'src/cod-tools/trunk/data/replacement-values/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 5376 2017-05-30 11:51:03Z andrius 
;
_cod_original_cell_volume        1084.19(14)
_cod_original_sg_symbol_H-M      Cc
_cod_database_code               7110886
loop_
_symmetry_equiv_pos_as_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'
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 0.87109(9) 0.87417(3) 0.09319(8) 0.02740(18) Uani 1 1 d D
H1G H 0.970(14) 0.889(5) -0.061(8) 0.11(4) Uiso 1 1 d D
H2G H 0.944(10) 0.848(3) 0.263(5) 0.054(19) Uiso 1 1 d D
Ga2 Ga 0.46280(8) 0.91624(3) 0.06414(7) 0.02886(19) Uani 1 1 d D
H3G H 0.344(9) 0.913(3) 0.212(6) 0.04(2) Uiso 1 1 d D
H4G H 0.412(12) 0.953(4) -0.098(6) 0.09(3) Uiso 1 1 d D
N1 N 0.7230(7) 0.9599(3) 0.1235(6) 0.0240(11) Uani 1 1 d .
H1N H 0.720(8) 0.970(3) 0.220(7) 0.014(15) Uiso 1 1 d .
N2 N 0.7708(8) 1.0174(3) 0.0212(6) 0.0287(12) Uani 1 1 d .
N3 N 0.6099(8) 0.8276(3) 0.0445(7) 0.0292(12) Uani 1 1 d .
H3N H 0.611(12) 0.810(4) -0.045(10) 0.06(3) Uiso 1 1 d .
N4 N 0.5774(8) 0.7737(2) 0.1613(6) 0.0317(12) Uani 1 1 d .
C1 C 0.9762(11) 1.0372(3) 0.0619(9) 0.0354(14) Uani 1 1 d .
H1A H 1.0618 0.9995 0.0356 0.08(3) Uiso 1 1 calc R
H1B H 0.9982 1.0479 0.1803 0.027(15) Uiso 1 1 calc R
H1C H 1.0057 1.0774 -0.0032 0.036(18) Uiso 1 1 calc R
C2 C 0.6422(10) 1.0749(4) 0.0517(8) 0.0356(16) Uani 1 1 d .
H2A H 0.5056 1.0617 0.0225 0.013(14) Uiso 1 1 calc R
H2B H 0.6749 1.1139 -0.0162 0.025(17) Uiso 1 1 calc R
H2C H 0.6603 1.0875 0.1693 0.07(3) Uiso 1 1 calc R
C3 C 0.7112(11) 0.7171(3) 0.1338(9) 0.0439(18) Uani 1 1 d .
H3A H 0.8469 0.7331 0.1515 0.06(2) Uiso 1 1 calc R
H3B H 0.6850 0.7003 0.0199 0.09(3) Uiso 1 1 calc R
H3C H 0.6908 0.6801 0.2118 0.07(2) Uiso 1 1 calc R
C4 C 0.3732(10) 0.7502(4) 0.1345(8) 0.0426(18) Uani 1 1 d .
H4A H 0.2856 0.7864 0.1665 0.07(3) Uiso 1 1 calc R
H4B H 0.3562 0.7096 0.2020 0.032(15) Uiso 1 1 calc R
H4C H 0.3419 0.7391 0.0170 0.05(2) Uiso 1 1 calc R
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ga1 0.0269(4) 0.0246(4) 0.0304(3) 0.0010(3) 0.0013(3) -0.0014(3)
Ga2 0.0264(4) 0.0272(4) 0.0327(4) 0.0015(3) 0.0013(3) -0.0029(3)
N1 0.030(3) 0.026(3) 0.016(3) 0.002(2) 0.003(2) -0.008(2)
N2 0.040(3) 0.019(3) 0.027(3) 0.000(2) 0.002(2) -0.003(2)
N3 0.035(3) 0.022(3) 0.031(3) 0.005(3) 0.004(2) -0.004(3)
N4 0.040(3) 0.023(3) 0.031(3) 0.009(2) -0.002(2) -0.006(2)
C1 0.039(4) 0.028(3) 0.037(3) 0.001(4) -0.006(3) -0.009(4)
C2 0.041(4) 0.023(4) 0.043(4) -0.001(3) 0.003(3) 0.003(3)
C3 0.050(5) 0.027(4) 0.053(4) 0.003(4) -0.006(4) 0.001(4)
C4 0.043(4) 0.038(4) 0.048(4) 0.012(3) 0.008(4) -0.014(4)
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'
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
N1 Ga1 N3 87.3(2)
N1 Ga1 Ga2 43.28(14)
N3 Ga1 Ga2 44.07(16)
N1 Ga1 H1G 102(4)
N3 Ga1 H1G 113(4)
Ga2 Ga1 H1G 113(4)
N1 Ga1 H2G 108(2)
N3 Ga1 H2G 104(3)
Ga2 Ga1 H2G 114(3)
H1G Ga1 H2G 133(5)
N1 Ga2 N3 86.9(2)
N1 Ga2 Ga1 43.10(16)
N3 Ga2 Ga1 43.88(15)
N1 Ga2 H3G 111(3)
N3 Ga2 H3G 110(2)
Ga1 Ga2 H3G 121(3)
N1 Ga2 H4G 98(3)
N3 Ga2 H4G 115(3)
Ga1 Ga2 H4G 111(3)
H3G Ga2 H4G 128(4)
N2 N1 Ga1 116.1(4)
N2 N1 Ga2 116.0(4)
Ga1 N1 Ga2 93.6(2)
N2 N1 H1N 113(4)
Ga1 N1 H1N 113(4)
Ga2 N1 H1N 103(4)
N1 N2 C2 109.2(5)
N1 N2 C1 109.8(5)
C2 N2 C1 109.8(5)
N4 N3 Ga1 113.0(4)
N4 N3 Ga2 117.8(4)
Ga1 N3 Ga2 92.1(2)
N4 N3 H3N 108(6)
Ga1 N3 H3N 107(6)
Ga2 N3 H3N 119(6)
N3 N4 C3 108.4(6)
N3 N4 C4 109.5(5)
C3 N4 C4 109.9(5)
N2 C1 H1A 109.5
N2 C1 H1B 109.5
H1A C1 H1B 109.5
N2 C1 H1C 109.5
H1A C1 H1C 109.5
H1B C1 H1C 109.5
N2 C2 H2A 109.5
N2 C2 H2B 109.5
H2A C2 H2B 109.5
N2 C2 H2C 109.5
H2A C2 H2C 109.5
H2B C2 H2C 109.5
N4 C3 H3A 109.5
N4 C3 H3B 109.5
H3A C3 H3B 109.5
N4 C3 H3C 109.5
H3A C3 H3C 109.5
H3B C3 H3C 109.5
N4 C4 H4A 109.5
N4 C4 H4B 109.5
H4A C4 H4B 109.5
N4 C4 H4C 109.5
H4A C4 H4C 109.5
H4B C4 H4C 109.5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Ga1 N1 1.991(5)
Ga1 N3 2.017(5)
Ga1 Ga2 2.9076(9)
Ga1 H1G 1.51(3)
Ga1 H2G 1.51(3)
Ga2 N1 1.997(5)
Ga2 N3 2.024(6)
Ga2 H3G 1.51(3)
Ga2 H4G 1.51(3)
N1 N2 1.454(7)
N1 H1N 0.81(5)
N2 C2 1.466(8)
N2 C1 1.469(8)
N3 N4 1.449(7)
N3 H3N 0.80(8)
N4 C3 1.470(9)
N4 C4 1.471(8)
C1 H1A 0.9800
C1 H1B 0.9800
C1 H1C 0.9800
C2 H2A 0.9800
C2 H2B 0.9800
C2 H2C 0.9800
C3 H3A 0.9800
C3 H3B 0.9800
C3 H3C 0.9800
C4 H4A 0.9800
C4 H4B 0.9800
C4 H4C 0.9800
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1N N2 0.81(5) 2.45(5) 3.238(7) 167(5) 2_575
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
N3 Ga1 Ga2 N1 176.0(3)
N1 Ga1 Ga2 N3 -176.0(3)
N3 Ga1 N1 N2 -124.2(4)
Ga2 Ga1 N1 N2 -121.4(4)
N3 Ga1 N1 Ga2 -2.8(2)
N3 Ga2 N1 N2 124.2(4)
Ga1 Ga2 N1 N2 121.4(5)
N3 Ga2 N1 Ga1 2.8(2)
Ga1 N1 N2 C2 176.9(4)
Ga2 N1 N2 C2 68.4(5)
Ga1 N1 N2 C1 -62.7(5)
Ga2 N1 N2 C1 -171.2(4)
N1 Ga1 N3 N4 -118.8(4)
Ga2 Ga1 N3 N4 -121.5(5)
N1 Ga1 N3 Ga2 2.8(2)
N1 Ga2 N3 N4 114.7(4)
Ga1 Ga2 N3 N4 117.4(5)
N1 Ga2 N3 Ga1 -2.7(2)
Ga1 N3 N4 C3 -69.4(5)
Ga2 N3 N4 C3 -175.0(4)
Ga1 N3 N4 C4 170.7(4)
Ga2 N3 N4 C4 65.1(6)
