#------------------------------------------------------------------------------
#$Date: 2016-03-21 10:45:35 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178666 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/77/4077749.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_4077749
loop_
_publ_author_name
'Jutzi, Peter'
'Neumann, Beate'
'Reumann, Guido'
'Stammler, Hans-Georg'
_publ_section_title
;
 Novel Ga2N2Ring Systems by Reaction of Pentamethylcyclopentadienylgallium
 with Organic Azides
;
_journal_issue                   10
_journal_name_full               Organometallics
_journal_page_first              2037
_journal_paper_doi               10.1021/om980944l
_journal_volume                  18
_journal_year                    1999
_chemical_formula_sum            'C36 H48 Ga2 N2'
_chemical_formula_weight         648.20
_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                 104.84(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.788(3)
_cell_length_b                   9.086(2)
_cell_length_c                   14.702(3)
_cell_measurement_temperature    173(2)
_cell_volume                     1651.3(6)
_computing_cell_refinement       'P3 (1989)'
_computing_data_collection       'P3 (1989)'
_computing_data_reduction        'SHELXTL-PLUS (1990)'
_computing_molecular_graphics    'SHELXTL-PLUS (1990)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.944
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measurement_device       'Siemens P2(1) diffractometer'
_diffrn_measurement_method       Wyckoff-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  0.0153
_diffrn_reflns_av_sigmaI/netI    0.0532
_diffrn_refln_scan_width         1.6
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            5162
_diffrn_reflns_theta_full        29.99
_diffrn_reflns_theta_max         29.99
_diffrn_reflns_theta_min         2.78
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.657
_exptl_absorpt_correction_T_max  0.6362
_exptl_absorpt_correction_T_min  0.4912
_exptl_absorpt_correction_type   'semi-empirical from psi-scans'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.304
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rhombic
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.351
_refine_diff_density_min         -0.467
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     188
_refine_ls_number_reflns         4805
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0708
_refine_ls_R_factor_gt           0.0410
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0366P)²+0.5891P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0823
_refine_ls_wR_factor_ref         0.0916
_reflns_number_gt                3521
_reflns_number_total             4805
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om980944l.cif
_cod_data_source_block           compound2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic ' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from
2011-04-26.

'_geom_bond_publ_flag' value 'Y' changed to 'y'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26 (25
times).

'_geom_angle_publ_flag' value 'Y' changed to 'y' according
to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary
named 'cif_core.dic' version 2.4.2 from 2011-04-26 (46 times).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0366P)^2^+0.5891P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0366P)^2^+0.5891P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4077749
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_calc_flag
_atom_site_refinement_flags
Ga1 Ga 0.037746(19) 0.08810(3) 0.944006(17) 0.02200(8) Uani 1 d .
N1 N -0.08958(15) 0.0760(2) 0.98396(14) 0.0256(4) Uani 1 d .
C1 C 0.09325(18) 0.2413(3) 0.87257(16) 0.0248(5) Uani 1 d .
C2 C 0.1542(2) 0.1486(3) 0.82114(17) 0.0274(5) Uani 1 d .
C3 C 0.25735(19) 0.1322(3) 0.87530(18) 0.0304(5) Uani 1 d .
C4 C 0.26994(19) 0.2180(3) 0.96058(18) 0.0323(6) Uani 1 d .
C5 C 0.1751(2) 0.2875(3) 0.95928(16) 0.0292(5) Uani 1 d .
C6 C 0.0069(2) 0.3477(3) 0.82009(19) 0.0370(6) Uani 1 d .
H6A H -0.0336 0.3860 0.8632 0.055 Uiso 1 calc R
H6B H -0.0426 0.2962 0.7679 0.055 Uiso 1 calc R
H6C H 0.0414 0.4295 0.7954 0.055 Uiso 1 calc R
C7 C 0.1044(2) 0.0876(4) 0.72495(18) 0.0409(6) Uani 1 d .
H7A H 0.0993 0.1656 0.6779 0.061 Uiso 1 calc R
H7B H 0.0319 0.0499 0.7224 0.061 Uiso 1 calc R
H7C H 0.1496 0.0074 0.7117 0.061 Uiso 1 calc R
C8 C 0.3443(2) 0.0352(4) 0.8557(2) 0.0481(8) Uani 1 d .
H8A H 0.3149 -0.0210 0.7979 0.072 Uiso 1 calc R
H8B H 0.3700 -0.0329 0.9084 0.072 Uiso 1 calc R
H8C H 0.4046 0.0962 0.8480 0.072 Uiso 1 calc R
C9 C 0.3724(2) 0.2204(4) 1.0386(2) 0.0543(9) Uani 1 d .
H9A H 0.3653 0.2921 1.0865 0.081 Uiso 1 calc R
H9B H 0.4333 0.2483 1.0131 0.081 Uiso 1 calc R
H9C H 0.3855 0.1225 1.0672 0.081 Uiso 1 calc R
C10 C 0.1502(3) 0.3897(3) 1.0319(2) 0.0436(7) Uani 1 d .
H10A H 0.0883 0.3516 1.0524 0.065 Uiso 1 calc R
H10B H 0.1329 0.4878 1.0044 0.065 Uiso 1 calc R
H10C H 0.2133 0.3962 1.0861 0.065 Uiso 1 calc R
C11 C -0.19177(19) 0.1414(3) 0.95256(17) 0.0265(5) Uani 1 d .
C12 C -0.2305(2) 0.2378(3) 1.01170(19) 0.0327(6) Uani 1 d .
C13 C -0.3310(2) 0.3035(3) 0.9780(2) 0.0453(7) Uani 1 d .
H13 H -0.3576 0.3687 1.0174 0.054 Uiso 1 calc R
C14 C -0.3931(2) 0.2752(4) 0.8877(3) 0.0517(9) Uani 1 d .
H14 H -0.4616 0.3213 0.8655 0.062 Uiso 1 calc R
C15 C -0.3559(2) 0.1808(4) 0.8302(2) 0.0448(8) Uani 1 d .
H15 H -0.3993 0.1618 0.7685 0.054 Uiso 1 calc R
C16 C -0.2555(2) 0.1122(3) 0.86082(18) 0.0331(6) Uani 1 d .
C17 C -0.1634(2) 0.2685(4) 1.1097(2) 0.0460(7) Uani 1 d .
H17A H -0.1982 0.3457 1.1382 0.069 Uiso 1 calc R
H17B H -0.0912 0.3013 1.1073 0.069 Uiso 1 calc R
H17C H -0.1571 0.1786 1.1476 0.069 Uiso 1 calc R
C18 C -0.2167(2) 0.0065(4) 0.7982(2) 0.0478(8) Uani 1 d .
H18A H -0.2753 -0.0133 0.7420 0.072 Uiso 1 calc R
H18B H -0.1944 -0.0857 0.8322 0.072 Uiso 1 calc R
H18C H -0.1550 0.0494 0.7796 0.072 Uiso 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'
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
N1 Ga1 N1 89.18(8) 3_557 . y
N1 Ga1 C1 138.15(9) 3_557 . y
N1 Ga1 C1 131.82(9) . . y
N1 Ga1 C5 113.15(9) 3_557 . y
N1 Ga1 C5 131.64(9) . . y
C1 Ga1 C5 36.63(8) . . y
N1 Ga1 Ga1 44.90(6) 3_557 3_557 y
N1 Ga1 Ga1 44.29(6) . 3_557 y
C1 Ga1 Ga1 172.24(7) . 3_557 y
C5 Ga1 Ga1 138.04(6) . 3_557 y
C11 N1 Ga1 134.21(16) . 3_557 y
C11 N1 Ga1 133.20(16) . . y
Ga1 N1 Ga1 90.82(8) 3_557 .. y
C2 C1 C5 104.6(2) . . y
C2 C1 C6 120.7(2) . . y
C5 C1 C6 121.0(2) . . y
C2 C1 Ga1 100.28(16) . . y
C5 C1 Ga1 90.76(14) . . y
C6 C1 Ga1 113.81(16) . . y
C3 C2 C1 108.7(2) . . y
C3 C2 C7 128.5(2) . . y
C1 C2 C7 122.7(2) . . y
C2 C3 C4 108.8(2) . . y
C2 C3 C8 127.2(3) . . y
C4 C3 C8 123.9(2) . . y
C5 C4 C3 109.6(2) . . y
C5 C4 C9 127.0(3) . . y
C3 C4 C9 123.3(3) . . y
C4 C5 C1 108.0(2) . . y
C4 C5 C10 128.5(2) . . y
C1 C5 C10 123.4(2) . . y
C4 C5 Ga1 105.57(18) . . y
C1 C5 Ga1 52.61(11) . . y
C10 C5 Ga1 103.87(16) . . y
N1 C11 C12 120.3(2) . . y
N1 C11 C16 119.8(2) . . y
C12 C11 C16 119.9(2) . . y
C13 C12 C11 119.1(3) . . y
C13 C12 C17 120.8(3) . . y
C11 C12 C17 120.2(2) . . y
C14 C13 C12 120.9(3) . . y
C15 C14 C13 120.2(3) . . y
C14 C15 C16 121.1(3) . . y
C15 C16 C11 118.9(3) . . y
C15 C16 C18 120.7(3) . . y
C11 C16 C18 120.4(2) . . y
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 N1 1.850(2) 3_557 y
Ga1 N1 1.8704(19) . y
Ga1 C1 1.981(2) . y
Ga1 C5 2.493(2) . y
Ga1 Ga1 2.6495(6) 3_557 y
N1 C11 1.402(3) . y
N1 Ga1 1.850(2) 3_557 y
C1 C2 1.479(3) . y
C1 C5 1.488(3) . y
C1 C6 1.521(3) . y
C2 C3 1.364(3) . y
C2 C7 1.500(3) . y
C3 C4 1.450(4) . y
C3 C8 1.503(4) . y
C4 C5 1.363(4) . y
C4 C9 1.505(3) . y
C5 C10 1.509(4) . y
C11 C12 1.410(4) . y
C11 C16 1.411(3) . y
C12 C13 1.389(4) . y
C12 C17 1.502(4) . y
C13 C14 1.385(5) . y
C14 C15 1.372(5) . y
C15 C16 1.394(4) . y
C16 C18 1.500(4) . y
