Synthesis and Photophysical Properties of Aza[n]helicenes.
Upadhyay, Gourav M.; Talele, Harish R.; Bedekar, Ashutosh V.; The Journal of organic chemistry 81 (2016) 7751–7759; doi:10.1021/acs.joc.6b01395

data_4037059
_publ_section_title
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 Synthesis and Photophysical Properties of Aza[n]helicenes.
;
_journal_issue                   17
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              7751
_journal_page_last               7759
_journal_paper_doi               10.1021/acs.joc.6b01395
_journal_volume                  81
_journal_year                    2016
_chemical_formula_moiety         'C40 H27 N'
_chemical_formula_sum            'C40 H27 N'
_chemical_formula_weight         521.63
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_cell_angle_alpha                90
_cell_angle_beta                 92.0494(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.33994(19)
_cell_length_b                   22.1450(3)
_cell_length_c                   8.96791(14)
_cell_measurement_temperature    293(2)
_cell_volume                     2647.54(7)
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.9936
_diffrn_measured_fraction_theta_max 0.9936
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0255
_diffrn_reflns_av_unetI/netI     0.0240
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            15884
_diffrn_reflns_theta_full        73.2168
_diffrn_reflns_theta_max         73.22
_diffrn_reflns_theta_min         3.32
_exptl_absorpt_coefficient_mu    0.572
_exptl_crystal_density_diffrn    1.3087
_exptl_crystal_F_000             1099.0493
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.2069
_refine_diff_density_min         -0.2389
_refine_diff_density_rms         0.0392
_refine_ls_d_res_high            0.8052
_refine_ls_d_res_low             13.3314
_refine_ls_goodness_of_fit_ref   1.0332
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    49
_refine_ls_number_parameters     370
_refine_ls_number_reflns         5317
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0332
_refine_ls_R_factor_all          0.0589
_refine_ls_R_factor_gt           0.0484
_refine_ls_shift/su_max          0.0051
_refine_ls_shift/su_mean         0.0009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0824P)^2^+0.3272P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1459
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              16
_reflns_limit_h_min              -16
_reflns_limit_k_max              27
_reflns_limit_k_min              0
_reflns_limit_l_max              11
_reflns_limit_l_min              0
_reflns_number_gt                4266
_reflns_number_total             5283
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            jo6b01395_si_002.cif
_cod_data_source_block           exp_679
_cod_original_cell_volume        2647.55(7)
_cod_database_code               4037059
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  H3 of C3, H18 of C18, H20 of C20, H21 of C21, H23 of C23, H24 of C24, H26
  of C26, H27 of C27, H28 of C28, {H29a,H29b} of C29, H30 of C30, H31 of C31,
  H32 of C32, H33 of C33, H34 of C34, H35 of C35, {H36a,H36b} of C36, H37 of
  C37, H38 of C38, H39 of C39, {H40a,H40b} of C40
 At 1.5 times of:
  {H41a,H41b,H41c} of C41
2.a Secondary CH2 refined with riding coordinates:
 C29(H29a,H29b), C36(H36a,H36b), C40(H40a,H40b)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C18(H18), C20(H20), C21(H21), C23(H23), C24(H24), C26(H26), C27(H27),
 C28(H28), C30(H30), C31(H31), C32(H32), C33(H33), C34(H34), C35(H35), C37(H37),
  C38(H38), C39(H39)
2.c Idealised Me refined as rotating group:
 C41(H41a,H41b,H41c)
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