Monochloroindium derivative of tmtaa (dibenzotetramethyltetraaza[14]annulene), [In(C~22~H~22~N~4~)Cl]
Phillips, Paul R.; McCamley, Andrew; Alcock, Nathaniel W.; Wallbridge, Malcolm G.H.; Acta Crystallographica Section C 50 (1994) 1072–1074; doi:10.1107/S0108270194000417

data_2009827
_publ_section_title
;
 Monochloroindium derivative of tmtaa
 (dibenzotetramethyltetraaza[14]annulene), [In(C~22~H~22~N~4~)Cl]
;
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1072
_journal_page_last               1074
_journal_paper_doi               10.1107/S0108270194000417
_journal_volume                  50
_journal_year                    1994
_chemical_formula_moiety         '[In(C~22~H~22~N~4~)Cl]'
_chemical_formula_sum            'C22 H22 Cl In N4'
_chemical_formula_weight         492.71
_chemical_name_systematic
;
 Monochloroindium 1,8-dihydro-5,7,12,14-tetramethyldibenzo[b,i][1,4,8,11]
tetraazacyclotetradecane
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 101.34(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.927(4)
_cell_length_b                   22.457(7)
_cell_length_c                   10.209(3)
_cell_measurement_reflns_used    16
_cell_measurement_temperature    220(2)
_cell_measurement_theta_max      9
_cell_measurement_theta_min      8
_cell_volume                     2006.7(13)
_computing_cell_refinement       'Siemens R3m system'
_computing_data_collection       'Siemens R3m system'
_computing_data_reduction        'SHELXTL-Plus (Sheldrick, 1991)'
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1994)'
_computing_structure_solution    'SHELXTL-Plus (Sheldrick, 1991)'
_diffrn_ambient_temperature      220(2)
_diffrn_measurement_device       'Siemens R3m'
_diffrn_measurement_method       \w-2\q
_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  0.0417
_diffrn_reflns_av_sigmaI/netI    0.0461
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            3700
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.81
_diffrn_standards_decay_%        8
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.33
_exptl_absorpt_correction_T_max  0.86
_exptl_absorpt_correction_T_min  0.81
_exptl_absorpt_correction_type   analytical
_exptl_crystal_colour            dark-orange
_exptl_crystal_density_diffrn    1.631
_exptl_crystal_description       blocks
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.860
_refine_diff_density_min         -1.454
_refine_ls_extinction_coef       0.0023(6)
_refine_ls_extinction_method     'SHELXL93 (Sheldrick, 1994)'
_refine_ls_goodness_of_fit_all   1.059
_refine_ls_goodness_of_fit_obs   1.038
_refine_ls_hydrogen_treatment    'H-atom parameters fixed'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     266
_refine_ls_number_reflns         3457
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.172
_refine_ls_restrained_S_obs      1.038
_refine_ls_R_factor_all          0.0727
_refine_ls_R_factor_obs          0.0464
_refine_ls_shift/esd_max         -0.025
_refine_ls_shift/esd_mean        0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0700P)^2^ +6.3000P] whereP=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1457
_refine_ls_wR_factor_obs         0.1121
_reflns_number_observed          2672
_reflns_number_total             3472
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ab1129.cif
_cod_data_source_block           macinzab
_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 2.4.1 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:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 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 'calc
w=1/[\s^2^(Fo^2^)+(0.0700P)^2^ +6.3000P] whereP=(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^)+(0.0700P)^2^ +6.3000P] whereP=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2006.7(12)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2009827