Crystal structure determination of <i>rac</i>-11'-(1-acetyl-1<i>H</i>-indazol-3-yl)-11',11<i>a</i>'-dihydro-10'<i>H</i>,17'<i>H</i>-spiro[indene-2,18'-[5a,16<i>b</i>]methanotriindeno[1,2-<i>b</i>:1',2'-<i>d</i>:2'',1''-<i>g</i>]oxocine]-1,3,10',12',17'(10<i>a</i>'<i>H</i>)-pentaone acetonitrile 1.5-solvate
Baranov, Mark; Vainer, Radion; Sigalov, Mark V.; Acta Crystallographica Section E 74 (2018) 1444–1447; doi:10.1107/S2056989018011763

data_2242643
_publ_section_title
;
 Crystal structure determination of
 <i>rac</i>-11'-(1-acetyl-1<i>H</i>-indazol-3-yl)-11',11<i>a</i>'-dihydro-10'<i>H</i>,17'<i>H</i>-spiro[indene-2,18'-[5a,16<i>b</i>]methanotriindeno[1,2-<i>b</i>:1',2'-<i>d</i>:2'',1''-<i>g</i>]oxocine]-1,3,10',12',17'(10<i>a</i>'<i>H</i>)-pentaone
 acetonitrile 1.5-solvate
;
_journal_coeditor_code           ZQ2241
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1444
_journal_page_last               1447
_journal_paper_doi               10.1107/S2056989018011763
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac          'C46 H26 N2 O7, 1.5C2 H3 N'
_chemical_formula_moiety         'C46 H26 N2 O7, 1.5(C2 H3 N)'
_chemical_formula_sum            'C49 H30.5 N3.5 O7'
_chemical_formula_weight         390.132
_chemical_name_systematic
'<i>rac</i>-11'-(1-Acetyl-1<i>H</i>-indazol-3-yl)-11',11a'-dihydro-10'<i>H</i>,17'<i>H</i>-spiro[indene-2,18'-[5a,16b]methanotriindeno[1,2-<i>b</i>:1',2'-<i>d</i>:2'',1''-<i>g</i>]oxocine]-1,3,10',12',17'(10a'<i>H</i>)-pentaone acetonitrile 1.5-solvate'
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 92.475(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.5195(3)
_cell_length_b                   13.0697(3)
_cell_length_c                   42.9248(9)
_cell_measurement_reflns_used    32475
_cell_measurement_temperature    99.99(16)
_cell_measurement_theta_max      25.1310
_cell_measurement_theta_min      2.3880
_cell_volume                     7577.6(3)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2018)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2018)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2018)
;
_computing_molecular_graphics
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009)
;
_computing_publication_material
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'Rigaku Oxford Diffraction XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0497
_diffrn_reflns_av_unetI/netI     0.0301
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            81627
_diffrn_reflns_theta_full        24.977
_diffrn_reflns_theta_max         24.977
_diffrn_reflns_theta_min         2.206
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.093
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72253
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2018)
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_density_diffrn    1.368
_exptl_crystal_description       cube
_exptl_crystal_F_000             3240
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.29
_refine_diff_density_max         1.149
_refine_diff_density_min         -0.429
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1077
_refine_ls_number_reflns         13290
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0574
_refine_ls_R_factor_gt           0.0471
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0537P)^2^+7.2184P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1167
_refine_ls_wR_factor_ref         0.1221
_reflns_number_gt                11196
_reflns_number_total             13290
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            zq2241sup1.cif
_cod_data_source_block           I
_cod_depositor_comments
;

2019-09-06
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_moiety     '2(C46 H26 N2 O7), 3(C2 H3 N)'
_cod_original_formula_sum        'C98 H61 N7 O14'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     780.265
_cod_database_code               2242643
_cod_database_fobs_code          2242643
_shelx_estimated_absorpt_t_min   0.973
_shelx_estimated_absorpt_t_max   0.973