2,12-Dichloro-10,20-diphenyl-5,7,15,17-tetrahydro-6<i>H</i>,16<i>H</i>-dibenzo[<i>d</i>,<i>l</i>][1,9,2,6,10,14]dioxotetraazacyclohexadecine-6,16-dione dioxane solvate as a potential macrocyclic hexadentate ligand
Khrustalev, Victor N.; Komissarov, Eugene A.; Kulikov, Oleg V.; Acta Crystallographica Section C 63 (2007) o374–o377; doi:10.1107/S0108270107021415

data_2016056
_publ_section_title
;2,12-Dichloro-10,20-diphenyl-5,7,15,17-tetrahydro-6<i>H</i>,16<i>H</i>-dibenzo[<i>d</i>,<i>l</i>][1,9,2,6,10,14]dioxotetraazacyclohexadecine-6,16-dione
 dioxane solvate as a potential macrocyclic hexadentate ligand
;
_journal_coeditor_code           LN3049
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o374
_journal_page_last               o377
_journal_paper_doi               10.1107/S0108270107021415
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C30 H22 Cl2 N4 O4 , C4 H8 O2'
_chemical_formula_moiety         'C30 H22 Cl2 N4 O4 , C4 H8 O2'
_chemical_formula_sum            'C34 H30 Cl2 N4 O6'
_chemical_formula_weight         661.52
_chemical_name_systematic
;
2,12-Dichloro-10,20-diphenyl-5,7,15,17-tetrahydro-6<i>H</i>,16<i>H</i>-
dibenzo[d,l][1,9,2,6,10,14]dioxotetraazacyclohexadecine-6,16-dione dioxane
solvate
;
_space_group_IT_number           2
_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           SHELXL97
_cell_angle_alpha                92.389(2)
_cell_angle_beta                 99.896(3)
_cell_angle_gamma                92.476(2)
_cell_formula_units_Z            4
_cell_length_a                   9.6834(6)
_cell_length_b                   14.2960(8)
_cell_length_c                   22.2970(13)
_cell_measurement_reflns_used    8835
_cell_measurement_temperature    120.0(2)
_cell_measurement_theta_max      28.0
_cell_measurement_theta_min      2.2
_cell_volume                     3034.1(3)
_computing_cell_refinement       'SAINT-Plus (Bruker, 1998)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        SAINT-Plus
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 1998)'
_diffrn_ambient_temperature      120.0(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0254
_diffrn_reflns_av_sigmaI/netI    0.0376
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            31338
_diffrn_reflns_theta_full        28.02
_diffrn_reflns_theta_max         28.02
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    0.269
_exptl_absorpt_correction_T_max  0.944
_exptl_absorpt_correction_T_min  0.928
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1998)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'orthogonal prism'
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.557
_refine_diff_density_min         -0.368
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     874
_refine_ls_number_reflns         14551
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0725
_refine_ls_R_factor_gt           0.0459
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.05P)^2^+2P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1065
_refine_ls_wR_factor_ref         0.1261
_reflns_number_gt                10236
_reflns_number_total             14551
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ln3049.cif
_cod_data_source_block           I
_cod_database_code               2016056
_cod_database_fobs_code          2016056