Metal assisted cyclodimerization of doubly N-confused dipyrrins into planar aza-heptalenes
Santosh C. Gadekar; Baddigam Kiran Reddy; Venkataramanarao G. Anand; Chem.Commun. 51 (2015) 8342–; doi:10.1039/C5cc01367D

data_7117125
_publ_section_title
;
 Metal assisted cyclodimerization of doubly N-confused dipyrrins into
 planar aza-heptalenes
;
_journal_name_full               Chem.Commun.
_journal_page_first              8342
_journal_paper_doi               10.1039/C5cc01367D
_journal_volume                  51
_journal_year                    2015
_chemical_formula_moiety         'C31 H10 F10 N4'
_chemical_formula_sum            'C31 H10 F10 N4'
_chemical_formula_weight         628.43
_chemical_name_systematic        '1N-Methyl Nornorrole'
_space_group_IT_number           1
_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
_audit_update_record
;
2014-09-16 deposited with the CCDC.
2015-04-07 downloaded from the CCDC.
;
_cell_angle_alpha                76.834(4)
_cell_angle_beta                 82.082(4)
_cell_angle_gamma                72.763(4)
_cell_formula_units_Z            1
_cell_length_a                   6.1461(11)
_cell_length_b                   7.3648(13)
_cell_length_c                   14.031(3)
_cell_measurement_temperature    100
_cell_volume                     588.95(19)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0319
_diffrn_reflns_av_sigmaI/netI    0.0517
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            14304
_diffrn_reflns_theta_full        33.96
_diffrn_reflns_theta_max         33.96
_diffrn_reflns_theta_min         1.49
_exptl_absorpt_coefficient_mu    0.162
_exptl_absorpt_correction_T_max  0.992
_exptl_absorpt_correction_T_min  0.981
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'multi-scan absorption correction'
_exptl_crystal_colour            Brown
_exptl_crystal_density_diffrn    1.772
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             314
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.813
_refine_diff_density_min         -0.321
_refine_diff_density_rms         0.079
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.1(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.963
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     407
_refine_ls_number_reflns         6749
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.963
_refine_ls_R_factor_all          0.0927
_refine_ls_R_factor_gt           0.0484
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0927P)^2^+0.2088P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1298
_refine_ls_wR_factor_ref         0.1616
_reflns_number_gt                4370
_reflns_number_total             9600
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5cc01367d2.cif
_cod_data_source_block           628
_cod_original_cell_volume        589.0(2)
_cod_database_code               7117125