Synthesis and crystal structure of tert-butyl (2′R,3R,3′R,4a′R,9a′S)-1-acetyl-5-chloro-3″-methyl-2,5″,9′-trioxo-1″-phenyl-1″,4a′,5″,9a′-tetrahydro-1′H,3′H,9′H-dispiro[indoline-3,4′-xanthene-2′,4″-pyrazole]-3′-carboxylate, C36H32ClN3O7
Li, Wu-Wu; Gu, Yuan-Zi; Cao, Lei; Zeitschrift für Kristallographie - New Crystal Structures 236 (2021) 77–80; doi:10.1515/ncrs-2020-0408

data_8104887
_publ_section_title
;
 Synthesis and crystal structure of tert-butyl
 (2&#x2032;R,3R,3&#x2032;R,4a&#x2032;R,9a&#x2032;S)-1-acetyl-5-chloro-3&#x2033;-methyl-2,5&#x2033;,9&#x2032;-trioxo-1&#x2033;-phenyl-1&#x2033;,4a&#x2032;,5&#x2033;,9a&#x2032;-tetrahydro-1&#x2032;H,3&#x2032;H,9&#x2032;H-dispiro[indoline-3,4&#x2032;-xanthene-2&#x2032;,4&#x2033;-pyrazole]-3&#x2032;-carboxylate,
 C36H32ClN3O7
;
_journal_issue                   1
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              77
_journal_page_last               80
_journal_paper_doi               10.1515/ncrs-2020-0408
_journal_volume                  236
_journal_year                    2021
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C36 H32 Cl N3 O7'
_chemical_formula_sum            'C36 H32 Cl N3 O7'
_chemical_formula_weight         654.09
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.4608(5)
_cell_length_b                   12.1489(5)
_cell_length_c                   23.1684(7)
_cell_measurement_reflns_used    5533
_cell_measurement_temperature    100.0(10)
_cell_measurement_theta_max      73.4380
_cell_measurement_theta_min      4.0690
_cell_volume                     3225.9(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.0(10)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0350
_diffrn_reflns_av_unetI/netI     0.0485
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            11377
_diffrn_reflns_point_group_measured_fraction_full 0.938
_diffrn_reflns_point_group_measured_fraction_max 0.892
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.322
_diffrn_reflns_theta_min         3.816
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.506
_exptl_absorpt_correction_T_max  1.506
_exptl_absorpt_correction_T_min  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 1999)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.347
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1368
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.706
_refine_diff_density_min         -0.496
_refine_diff_density_rms         0.069
_refine_ls_abs_structure_details
;
 Flack x determined using 1834 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.003(11)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     429
_refine_ls_number_reflns         5861
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0690
_refine_ls_R_factor_gt           0.0588
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0591P)^2^+4.8626P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1469
_refine_ls_wR_factor_ref         0.1546
_reflns_Friedel_coverage         0.661
_reflns_Friedel_fraction_full    0.872
_reflns_Friedel_fraction_max     0.809
_reflns_number_gt                5154
_reflns_number_total             5861
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2020-0408_suppl.cif
_cod_data_source_block           I
_cod_database_code               8104887