Synthesis, characterization, and rotational dynamics of crystalline molecular compasses with N-heterocyclic rotators.
Rodriguez-Molina, Braulio; Ochoa, Ma Eugenia; Farfán, Norberto; Santillan, Rosa; García-Garibay, Miguel A; The Journal of organic chemistry 74 (2009) 8554–8565; doi:10.1021/jo901261j

data_4029485
_publ_section_title
;
 Synthesis, characterization, and rotational dynamics of crystalline
 molecular compasses with N-heterocyclic rotators.
;
_journal_issue                   22
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              8554
_journal_page_last               8565
_journal_paper_doi               10.1021/jo901261j
_journal_volume                  74
_journal_year                    2009
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C46 H32 N2 O, C H Cl3'
_chemical_formula_sum            'C47 H33 Cl3 N2 O'
_chemical_formula_weight         748.1
_chemical_name_common            rsgen45
_chemical_name_systematic
;
 3,6-Bis(3,3,3-triphenylpropynyl)pyridazine N-oxide
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_date             2009-09-11T13:01:12-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 128.202(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.2312(5)
_cell_length_b                   18.3897(6)
_cell_length_c                   18.4657(6)
_cell_measurement_reflns_used    17708
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.91
_cell_measurement_wavelength     0.71073
_cell_volume                     3797.6(2)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Giacovazzo et al, 2004)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.882
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.25588E-1
_diffrn_orient_matrix_UB_12      0.419513E-1
_diffrn_orient_matrix_UB_13      -0.309227E-1
_diffrn_orient_matrix_UB_21      0.424198E-1
_diffrn_orient_matrix_UB_22      -0.338757E-1
_diffrn_orient_matrix_UB_23      -0.267727E-1
_diffrn_orient_matrix_UB_31      -0.516603E-1
_diffrn_orient_matrix_UB_32      -0.70373E-2
_diffrn_orient_matrix_UB_33      -0.554619E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.18
_diffrn_reflns_av_unetI/netI     0.1648
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            22614
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         27.07
_diffrn_reflns_theta_min         3.02
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.281
_exptl_absorpt_correction_T_max  0.9752
_exptl_absorpt_correction_T_min  0.9345
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs (Bruker)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.308
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.466
_refine_diff_density_min         -0.79
_refine_diff_density_rms         0.06
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     482
_refine_ls_number_reflns         7371
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.1999
_refine_ls_R_factor_gt           0.0961
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0681P)^2^+3.3977P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1945
_refine_ls_wR_factor_ref         0.2454
_reflns_number_gt                3493
_reflns_number_total             7371
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo901261j_si_005.cif
_cod_data_source_block           rsgen36-2
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4029485