Alkylated Trimethylene-Bridged Bis(p-Phenylenediamines)
Stephen F. Nelsen; Gaoquan Li; Kevin P. Schultz; Hieu Q. Tran; Ilia A. Guzei; Dennis H. Evans; Journal of the American Chemical Society 130 (2008) 11620–11622; doi:10.1021/ja802292g

data_4108259
_publ_contact_author_address
;
Department of Chemistry
University of Wisconsin-Madison
1101 University Ave
Madison, WI  53706
USA
;
_publ_contact_author_email       iguzei@chem.wisc.edu
_publ_contact_author_fax         608-262-0381
_publ_contact_author_name
;
Guzei, Ilia A. 
;
_publ_contact_author_phone       608-263-4694
_publ_section_title
;
 Alkylated Trimethylene-Bridged Bis(p-Phenylenediamines)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11620
_journal_page_last               11622
_journal_paper_doi               10.1021/ja802292g
_journal_volume                  130
_journal_year                    2008
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C22 H32 N4'
_chemical_formula_sum            'C22 H32 N4'
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_symmetry_space_group_name_H-M   'I b a 2'
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_audit_creation_method
;
manual editing of the CIF file 
created by SHELXTL Ver. 6.10
and processed with modiCIfer-03272007. 
;
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_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
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_cell_length_a                   17.3647(3)
_cell_length_b                   20.5552(4)
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_cell_measurement_reflns_used    9982
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      71.3062
_cell_measurement_theta_min      3.3317
_cell_volume                     3887.41(12)
_computing_cell_refinement       'SAINT Ver. 7.24A (Bruker-AXS, 2007)'
_computing_data_collection       'APEX Ver. 2.1-4 (Bruker-AXS, 2007)'
_computing_data_reduction        'SAINT Ver. 7.24A'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
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_computing_structure_solution    'SHELXTL (Bruker-AXS, 2007)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker SMART APEXII area detector'
_diffrn_measurement_method       '0.50\% \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           Mo-K\a
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_diffrn_reflns_av_R_equivalents  0.0273
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_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
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_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            22130
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_diffrn_reflns_theta_max         71.84
_diffrn_reflns_theta_min         3.33
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.554
_exptl_absorpt_correction_T_max  0.9467
_exptl_absorpt_correction_T_min  0.8172
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS  (Bruker-AXS, 2007)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.205
_exptl_crystal_description       needle
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.159
_refine_diff_density_min         -0.170
_refine_diff_density_rms         0.031
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.0(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     252
_refine_ls_number_reflns         3685
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.0314
_refine_ls_R_factor_gt           0.0297
_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^)+(0.0551P)^2^+0.9750P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0778
_refine_ls_wR_factor_ref         0.0793
_reflns_number_gt                3550
_reflns_number_total             3685
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja802292g_si_002.cif
_cod_data_source_block           nelsen14
_cod_original_sg_symbol_Hall     'I 2 -2c     '
_cod_original_sg_symbol_H-M      'I b a 2 '
_cod_database_code               4108259