#------------------------------------------------------------------------------
#$Date: 2022-09-28 18:08:17 +0300 (Wed, 28 Sep 2022) $
#$Revision: 278247 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/00/15/2001537.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# 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_2001537
loop_
_publ_author_name
'Alcock, N. W.'
'Blacker, N. C.'
'Errington, W.'
'Wallbridge, M. G. H.'
_publ_section_title
;
 Structure of the monomethylgallium derivative of TMTAA
 (dibenzotetramethyltetraaza[14]annulene)
;
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1359
_journal_page_last               1361
_journal_paper_doi               10.1107/S0108270193000484
_journal_volume                  49
_journal_year                    1993
_chemical_formula_sum            'C23 H25 Ga N4'
_chemical_formula_weight         472.2
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_type_scat_source           'SHELXTL-Plus (Sheldrick, 1986)'
_cell_angle_alpha                107.78(2)
_cell_angle_beta                 107.83(2)
_cell_angle_gamma                107.74(2)
_cell_formula_units_Z            2
_cell_length_a                   9.023(3)
_cell_length_b                   11.740(3)
_cell_length_c                   11.861(3)
_cell_measurement_reflns_used    20
_cell_measurement_temperature    290
_cell_measurement_theta_max      11
_cell_measurement_theta_min      9
_cell_volume                     1023.2(6)
_diffrn_measurement_device       'Siemens R3m'
_diffrn_measurement_method       ω-2θ
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3859
_diffrn_reflns_theta_max         25
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.4
_exptl_absorpt_correction_T_max  0.86
_exptl_absorpt_correction_T_min  0.78
_exptl_absorpt_correction_type   gaussian
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.39
_exptl_crystal_description       'irregular blocks'
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.5
_refine_diff_density_min         -0.5
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   0.84
_refine_ls_number_parameters     268
_refine_ls_number_reflns         2684
_refine_ls_R_factor_obs          0.053
_refine_ls_shift/esd_max         0.2
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[σ²(F)+gF²]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.060
_reflns_number_observed          2684
_reflns_number_total             3859
_reflns_observed_criterion       I/\s(I)>=2.0
_cod_data_source_file            hu1029.cif
_cod_data_source_block           hu1029_structure_1_of_1
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'Gaussian' changed to 'gaussian'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Gaussian' changed to
'gaussian' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

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 '1/[\s^2^(F)+gF^2^]' 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^(F)+gF^2^]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1023.3(5)
_cod_original_formula_sum        'C23 H25 Ga1 N4'
_cod_database_code               2001537
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x,-y,-z
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
Ga(1) .49431(8) .25098(6) .23528(5) .0340(10)
N(11) .4226(6) .0864(4) .2658(4) .036(2)
N(12) .2455(6) .2234(4) .1659(4) .036(2)
N(13) .5254(6) .4396(4) .2983(4) .040(2)
N(14) .6993(6) .3062(4) .4041(4) .035(2)
C(1) .2510(9) -.0812(7) .3170(6) .052(3)
C(2) .2710(7) .0184(5) .2608(5) .039(3)
C(3) .1253(7) .0405(5) .2109(5) .039(2)
C(4) .1109(7) .1364(6) .1670(5) .041(3)
C(5) -.0615(7) .1402(7) .1301(6) .049(3)
C(6) .6125(9) .6690(6) .4566(6) .050(3)
C(7) .6284(7) .5406(5) .4181(5) .036(2)
C(8) .7464(7) .5295(5) .5150(5) .040(2)
C(9) .7822(7) .4222(5) .5136(5) .037(2)
C(10) .9057(9) .4366(7) .6408(6) .057(3)
C(11) .5735(7) .0715(5) .3177(5) .036(3)
C(12) .7265(7) .1935(5) .3950(5) .035(2)
C(13) .8858(8) .1901(6) .4394(5) .043(3)
C(14) .8967(9) .0705(6) .4109(6) .049(3)
C(15) .7484(9) -.0475(6) .3328(6) .050(3)
C(16) .5876(8) -.0469(6) .2849(6) .044(3)
C(21) .2415(7) .3240(5) .1264(5) .037(3)
C(22) .1110(9) .3115(7) .0179(6) .055(3)
C(23) .1325(11) .4136(7) -.0189(7) .068(4)
C(24) .2823(10) .5275(7) .0491(7) .074(4)
C(25) .4168(9) .5419(6) .1571(6) .056(3)
C(26) .3950(8) .4420(6) .1972(5) .043(3)
C(30) .5539(9) .2115(6) .0869(6) .050(3)
H(1a) .3509(9) -.0468(7) .3990(6) ?
H(1b) .1494(9) -.0973(7) .3320(6) ?
H(1c) .2387(9) -.1630(7) .2559(6) ?
H(3a) .0202 -.0409 .1632 ?
H(5a) -.0431(7) .2313(7) .1638(6) ?
H(5b) -.1278(7) .0973(7) .0360(6) ?
H(5c) -.1236(7) .0950(7) .1683(6) ?
H(6a) .4907(9) .6448(6) .4168(6) ?
H(6b) .6590(9) .7178(6) .5504(6) ?
H(6c) .6701(9) .7234(6) .4228(6) ?
H(8a) .8158 .6089 .5967 ?
H(10a) .8932(9) .3585(7) .6548(6) ?
H(10b) 1.0191(9) .4784(7) .6467(6) ?
H(10c) .8911(9) .4975(7) .7069(6) ?
H(13a) .9899 .2722 .4910 ?
H(14a) 1.0073 .0698 .4456 ?
H(16a) .4850 -.1294 .2282 ?
H(22a) .0058 .2302 -.0333 ?
H(24a) .2956 .5985 .0231 ?
H(25a) .5253 .6205 .2032 ?
H(30a) .5889(9) .2900(6) .0732(6) ?
H(30b) .6470(9) .1862(6) .1053(6) ?
H(30c) .4542(9) .1404(6) .0090(6) ?
H(151) .7590(9) -.1449(6) .3041(6) ?
H(231) .0479(9) .4150(6) -.0876(6) ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
N(11) Ga(1) N(12) 89.6(2) yes
N(12) Ga(1) N(13) 78.7(2) yes
N(12) Ga(1) N(14) 141.4(2) yes
N(11) Ga(1) C(30) 108.6(3) yes
N(13) Ga(1) C(30) 107.7(3) yes
Ga(1) N(11) C(2) 127.5(5) yes
C(2) N(11) C(11) 125.1(6) yes
Ga(1) N(12) C(21) 106.5(4) yes
Ga(1) N(13) C(7) 128.2(5) yes
C(7) N(13) C(26) 124.6(6) yes
Ga(1) N(14) C(12) 106.9(3) yes
N(11) C(2) C(1) 120.9(6) yes
C(1) C(2) C(3) 116.5(6) yes
N(12) C(4) C(3) 121.7(6) yes
C(3) C(4) C(5) 115.6(6) yes
N(13) C(7) C(8) 121.8(6) yes
C(7) C(8) C(9) 130.6(4) yes
N(14) C(9) C(10) 121.0(6) yes
N(11) C(11) C(12) 114.0(5) yes
C(12) C(11) C(16) 119.2(6) yes
N(14) C(12) C(13) 126.4(5) yes
C(12) C(13) C(14) 121.0(5) yes
C(14) C(15) C(16) 120.3(7) yes
N(12) C(21) C(22) 126.4(5) yes
C(22) C(21) C(26) 118.6(6) yes
C(22) C(23) C(24) 120.8(8) yes
C(24) C(25) C(26) 119.8(6) yes
N(13) C(26) C(25) 125.3(5) yes
N(11) Ga(1) N(13) 143.8(2) yes
N(11) Ga(1) N(14) 78.8(2) yes
N(13) Ga(1) N(14) 89.3(2) yes
N(12) Ga(1) C(30) 108.2(2) yes
N(14) Ga(1) C(30) 110.4(3) yes
Ga(1) N(11) C(11) 106.4(4) yes
Ga(1) N(12) C(4) 128.4(5) yes
C(4) N(12) C(21) 124.8(6) yes
Ga(1) N(13) C(26) 106.5(3) yes
Ga(1) N(14) C(9) 128.0(5) yes
C(9) N(14) C(12) 124.5(5) yes
N(11) C(2) C(3) 122.6(6) yes
C(2) C(3) C(4) 129.2(6) yes
N(12) C(4) C(5) 122.5(6) yes
N(13) C(7) C(6) 121.4(5) yes
C(6) C(7) C(8) 116.7(4) yes
N(14) C(9) C(8) 121.0(5) yes
C(8) C(9) C(10) 117.8(5) yes
N(11) C(11) C(16) 126.1(4) yes
N(14) C(12) C(11) 114.2(5) yes
C(11) C(12) C(13) 118.9(6) yes
C(13) C(14) C(15) 119.8(7) yes
C(11) C(16) C(15) 120.7(5) yes
N(12) C(21) C(26) 114.5(5) yes
C(21) C(22) C(23) 120.5(5) yes
C(23) C(24) C(25) 119.9(8) yes
N(13) C(26) C(21) 113.9(6) yes
C(21) C(26) C(25) 120.3(6) yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Ga(1) N(11) 2.023(5) yes
Ga(1) N(13) 2.005(5) yes
Ga(1) C(30) 1.958(8) yes
N(11) C(11) 1.401(8) yes
N(12) C(21) 1.403(9) yes
N(13) C(26) 1.415(8) yes
N(14) C(12) 1.396(9) yes
C(2) C(3) 1.404(10) yes
C(4) C(5) 1.500(10) yes
C(7) C(8) 1.378(9) yes
C(9) C(10) 1.500(9) yes
C(11) C(16) 1.381(10) yes
C(13) C(14) 1.381(11) yes
C(15) C(16) 1.390(11) yes
C(21) C(26) 1.396(7) yes
C(23) C(24) 1.355(9) yes
C(25) C(26) 1.377(11) yes
Ga(1) N(12) 2.022(5) yes
Ga(1) N(14) 2.015(4) yes
N(11) C(2) 1.329(8) yes
N(12) C(4) 1.335(8) yes
N(13) C(7) 1.334(5) yes
N(14) C(9) 1.344(6) yes
C(1) C(2) 1.505(11) yes
C(3) C(4) 1.401(10) yes
C(6) C(7) 1.500(10) yes
C(8) C(9) 1.389(9) yes
C(11) C(12) 1.420(6) yes
C(12) C(13) 1.389(10) yes
C(14) C(15) 1.377(7) yes
C(21) C(22) 1.384(9) yes
C(22) C(23) 1.377(13) yes
C(24) C(25) 1.391(11) yes
