Hydrogen bonded dimers of triurea derivatives of triphenylmethanes.
Rudzevich, Yuliya; Rudzevich, Valentyn; Schollmeyer, Dieter; Thondorf, Iris; Böhmer, Volker; Organic letters 7 (2005) 613–616; doi:10.1021/ol0476265

data_1506471
_publ_section_title
;
 Hydrogen bonded dimers of triurea derivatives of triphenylmethanes.
;
_journal_issue                   4
_journal_name_full               'Organic letters'
_journal_page_first              613
_journal_page_last               616
_journal_paper_doi               10.1021/ol0476265
_journal_volume                  7
_journal_year                    2005
_chemical_formula_sum            'C31 H37 N3 O9'
_chemical_formula_weight         595.64
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_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                100.789(13)
_cell_angle_beta                 103.509(19)
_cell_angle_gamma                103.50(2)
_cell_formula_units_Z            2
_cell_length_a                   9.860(4)
_cell_length_b                   12.3513(18)
_cell_length_c                   13.171(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    193(2)
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_cell_measurement_theta_min      65
_cell_volume                     1466.1(7)
_computing_cell_refinement       'Enraf Nonius Software V5'
_computing_data_collection       'Enraf Nonius Software V5'
_computing_data_reduction        'Corinc (Dr\"ager, 1971)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-92 (Altomare, 1994)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'CAD4 Enraf Nonius'
_diffrn_measurement_method       \q/2\w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0619
_diffrn_reflns_av_sigmaI/netI    0.0231
_diffrn_reflns_limit_h_max       11
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_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
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_diffrn_reflns_theta_full        73.56
_diffrn_reflns_theta_max         73.56
_diffrn_reflns_theta_min         3.57
_diffrn_source                   'rotating anode'
_diffrn_standards_decay_%        5
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.828
_exptl_absorpt_correction_T_max  0.9489
_exptl_absorpt_correction_T_min  0.7081
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   'Corinc (Dr\"ager, 1971)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.349
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.799
_refine_diff_density_min         -0.410
_refine_diff_density_rms         0.098
_refine_ls_extinction_coef       0.0049(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     420
_refine_ls_number_reflns         5904
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0814
_refine_ls_R_factor_gt           0.0757
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1352P)^2^+0.8318P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.1977
_refine_ls_wR_factor_ref         0.2050
_reflns_number_gt                5249
_reflns_number_total             5904
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol0476265si20041118_074121.cif
_cod_data_source_block           4b
_cod_original_cell_volume        1466.1(6)
_cod_database_code               1506471