A new approach to the 8b-azaacenaphthylene ring system.
Kamath, Anushree; Fabritius, Charles-Henry; Philouze, Christian; Delair, Philippe; Organic & biomolecular chemistry 13 (2015) 9834–9843; doi:10.1039/c5ob01013f

data_7154644
_publ_section_title
;
 A new approach to the 8b-azaacenaphthylene ring system.
;
_journal_issue                   38
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              9834
_journal_page_last               9843
_journal_paper_doi               10.1039/c5ob01013f
_journal_volume                  13
_journal_year                    2015
_chemical_formula_moiety         'C37 H53 N O4'
_chemical_formula_sum            'C37 H53 N O4'
_chemical_formula_weight         575.80
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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_date             2015-05-18
_audit_creation_method
;
  Olex2 1.1
  (compiled Sep 28 2011 20:36:17, GUI svn.r3906)
;
_audit_update_record
;
2015-05-19 deposited with the CCDC.
2015-07-22 downloaded from the CCDC.
;
_cell_angle_alpha                103.176(13)
_cell_angle_beta                 92.751(15)
_cell_angle_gamma                74.496(15)
_cell_formula_units_Z            2
_cell_length_a                   8.3651(17)
_cell_length_b                   10.416(2)
_cell_length_c                   21.073(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    297
_cell_measurement_theta_max      21.716
_cell_measurement_theta_min      18.180
_cell_volume                     1722.6(6)
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_collection       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      297
_diffrn_detector                 'scintillation LiI'
_diffrn_detector_dtime           1.195
_diffrn_detector_type            'scintillation LiI'
_diffrn_measured_fraction_theta_full 0.946
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker-Enraf-Nonius CAD4'
_diffrn_measurement_method       'omega scans'
_diffrn_orient_matrix_type
;
  x-axis points to radiation source
  the matrix is specified in reciprocal space
;
_diffrn_orient_matrix_UB_11      -0.044286
_diffrn_orient_matrix_UB_12      0.012554
_diffrn_orient_matrix_UB_13      0.044876
_diffrn_orient_matrix_UB_21      0.021699
_diffrn_orient_matrix_UB_22      -0.101314
_diffrn_orient_matrix_UB_23      -0.006345
_diffrn_orient_matrix_UB_31      -0.113848
_diffrn_orient_matrix_UB_32      0.005170
_diffrn_orient_matrix_UB_33      -0.017934
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0290
_diffrn_reflns_av_unetI/netI     0.0345
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6911
_diffrn_reflns_theta_full        74.89
_diffrn_reflns_theta_max         75.00
_diffrn_reflns_theta_min         3.00
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_source_target            Cu
_diffrn_source_type              'fine-focus sealed tube'
_diffrn_standards_decay_%        8
_diffrn_standards_interval_time  120
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.552
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.110
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             628
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.208
_refine_diff_density_min         -0.182
_refine_diff_density_rms         0.050
_refine_ls_extinction_coef       0.0073(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   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     389
_refine_ls_number_reflns         6720
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.1091
_refine_ls_R_factor_gt           0.0617
_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^)+(0.1091P)^2^+0.3112P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1690
_refine_ls_wR_factor_ref         0.2104
_reflns_number_gt                4125
_reflns_number_total             6720
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ob01013f2.cif
_cod_data_source_block           protalc2
_cod_depositor_comments
'Adding full bibliography for 7154643--7154645.cif.'
_cod_original_cell_volume        1722.5(6)
_cod_database_code               7154644
_diffrn_standards_decay_corr_max 1.111
_diffrn_standards_decay_corr_min 0.926