Steering non-centrosymmetry into the third dimension: crystal engineering of an octupolar nonlinear optical crystal
Thalladi, Venkat R.; Boese, Roland; Brasselet, Sophie; Ledoux, Isabelle; Zyss, Joseph; Jetti, Ram K. R.; Desiraju, Gautam R.; Chemical Communications  (1999) 1639–; doi:10.1039/a904490f

data_7110616
_publ_section_title
;
 Steering non-centrosymmetry into the third dimension: crystal engineering
 of an octupolar nonlinear optical crystal
;
_journal_issue                   17
_journal_name_full               'Chemical Communications'
_journal_page_first              1639
_journal_paper_doi               10.1039/a904490f
_journal_year                    1999
_chemical_formula_moiety         'C24 H21 N3 O3'
_chemical_formula_sum            'C24 H21 N3 O3'
_chemical_formula_weight         399.44
_chemical_name_systematic
; 
 2,4,6-tris-(4-methylphenoxy)-1,3,5-triazine 
;
_space_group_IT_number           161
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  'R 3 -2"c'
_symmetry_space_group_name_H-M   'R 3 c :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   23.576(3)
_cell_length_b                   23.576(3)
_cell_length_c                   6.5913(8)
_cell_measurement_reflns_used    2710
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      28.24
_cell_measurement_theta_min      2.99
_cell_volume                     3172.8(7)
_computing_cell_refinement       'Siemens SAINT program Vers.4.050'
_computing_data_collection       'Siemens SMART CCD area detector system'
_computing_data_reduction        'Siemens SAINT program Vers.4.050'
_computing_molecular_graphics    'Siemens SHELXL-97 UNIX VERSION Release 97-1'
_computing_publication_material  'Siemens SHELXL-97 UNIX VERSION Release 97-1'
_computing_structure_refinement  'Siemens SHELXL-97 UNIX VERSION Release 97-1'
_computing_structure_solution    'Siemens SHELXTL Vers.5.03, SGI-Version'
_diffrn_ambient_temperature      223(2)
_diffrn_detector_area_resol_mean 512
_diffrn_measured_fraction_theta_full 0.266
_diffrn_measured_fraction_theta_max 0.266
_diffrn_measurement_device_type  'Siemens SMART CCD area detector system'
_diffrn_measurement_method
;
 Fullsphere data collection 
 in omega at 0.3 deg scan width, 120 frames, phi=0 deg 
 in phi at 0.3 deg scan width 
 four runs with 600 frames, omega = 135,143,156,169 (deg) 
;
_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  0.1420
_diffrn_reflns_av_sigmaI/netI    0.0448
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            8988
_diffrn_reflns_theta_full        28.24
_diffrn_reflns_theta_max         28.24
_diffrn_reflns_theta_min         2.99
_exptl_absorpt_coefficient_mu    0.084
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.349
_exptl_absorpt_correction_type   'empirical on equivalent reflections'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.254
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1260
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.280
_refine_diff_density_min         -0.238
_refine_diff_density_rms         0.071
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -2(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.137
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     91
_refine_ls_number_reflns         750
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.136
_refine_ls_R_factor_all          0.0615
_refine_ls_R_factor_gt           0.0584
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0943P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1274
_refine_ls_wR_factor_ref         0.1321
_reflns_number_gt                691
_reflns_number_total             750
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            904490fsup1.cif
_cod_data_source_block           1g
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0943P)^2^+0.0000P] 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^)+(0.0943P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3172.9(7)
_cod_original_sg_symbol_H-M      R3c
_cod_database_code               7110616