Hydrogen-bonded networks formed from tri- and tetra-substituted adamantanes bearing dimethoxyphenol moieties and their 1,3,5-trinitrobenzene complexes via charge-transfer interactions
Tominaga, Masahide; Katagiri, Kosuke; Azumaya, Isao; CrystEngComm 12 (2010) 1164–; doi:10.1039/b917654c

data_7211984
_publ_section_title
;
 Hydrogen-bonded networks formed from tri- and tetra-substituted
 adamantanes bearing dimethoxyphenol moieties and their
 1,3,5-trinitrobenzene complexes via charge-transfer interactions
;
_journal_issue                   4
_journal_name_full               CrystEngComm
_journal_page_first              1164
_journal_paper_doi               10.1039/b917654c
_journal_volume                  12
_journal_year                    2010
_chemical_formula_sum            'C55 H55 Cl3 N6 O24'
_chemical_formula_weight         1290.40
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                102.717(15)
_cell_angle_beta                 91.783(13)
_cell_angle_gamma                107.300(13)
_cell_formula_units_Z            2
_cell_length_a                   13.052(14)
_cell_length_b                   14.340(15)
_cell_length_c                   16.268(17)
_cell_measurement_reflns_used    2328
_cell_measurement_temperature    120
_cell_measurement_theta_max      0.00
_cell_measurement_theta_min      0.00
_cell_volume                     2820(5)
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT (Bruker AXS, 2004)'
_computing_molecular_graphics    'XSHEL (Bruker AXS,2002)'
_computing_publication_material  'XCIF (Bruker AXS, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.847
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0460
_diffrn_reflns_av_sigmaI/netI    0.1298
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            13258
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.99
_diffrn_reflns_theta_min         1.98
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.255
_exptl_absorpt_correction_T_max  0.9874
_exptl_absorpt_correction_T_min  0.9160
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS Sheldrick 1996
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.519
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1340
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.701
_refine_diff_density_min         -0.587
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     829
_refine_ls_number_reflns         10415
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.1627
_refine_ls_R_factor_gt           0.0785
_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/[\s^2^(Fo^2^)+(0.1325P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2009
_refine_ls_wR_factor_ref         0.2500
_reflns_number_gt                5247
_reflns_number_total             10415
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b917654c.txt
_cod_data_source_block           a0906221kka
_cod_depositor_comments
;
The following automatic conversions were performed:

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

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        2821(5)
_cod_original_sg_symbol_H-M      'P-1 '
_cod_database_code               7211984