A synchrotron study of (2<i>R</i>,5'<i>S</i>)-5'-benzyl-5-bromo-6-methoxyspiro[indane-2,2'-piperazine]-3',6'-dione dimethylformamide solvate
Nichol, Gary S.; Murigi, Francis N.; Mash, Eugene A.; Acta Crystallographica Section C 66 (2010) o302–o304; doi:10.1107/S0108270110017579

data_2017662
_publ_section_title
;
 A synchrotron study of
 (2<i>R</i>,5'<i>S</i>)-5'-benzyl-5-bromo-6-methoxyspiro[indane-2,2'-piperazine]-3',6'-dione
 dimethylformamide solvate
;
_journal_coeditor_code           EG3048
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o302
_journal_page_last               o304
_journal_paper_doi               10.1107/S0108270110017579
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C20 H19 Br1 N2 O3, C3 H7 N O'
_chemical_formula_moiety         'C20 H19 Br1 N2 O3, C3 H7 N O'
_chemical_formula_sum            'C23 H26 Br N3 O4'
_chemical_formula_weight         488.38
_chemical_name_systematic
;
(2<i>R</i>,5'<i>S</i>)-5'-benzyl-5-bromo-6-methoxyspiro[indane-2,2'-
piperazine]-3',6'-dione dimethylformamide solvate
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   difmap
_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                   6.0741(7)
_cell_length_b                   13.8336(16)
_cell_length_c                   26.076(3)
_cell_measurement_reflns_used    1876
_cell_measurement_temperature    100
_cell_measurement_theta_max      25
_cell_measurement_theta_min      3
_cell_volume                     2191.1(4)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics
'ORTEP3 for Windows (Farrugia, 1997) and Mercury (Macrae <i>et al.</i>,  2008)'
_computing_publication_material  'CRYSTALS (Betteridge <i>et al.</i>,  2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge <i>et al.</i>,  2003)'
_computing_structure_solution    'SIR92 (Altomare <i>et al.</i>,  1993)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Bruker SMART APEXII CCD diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEXII CCD diffractometer'
_diffrn_measurement_method       '0.3 degree \w scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7749
_diffrn_reflns_av_R_equivalents  0.057
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            31454
_diffrn_reflns_theta_full        29.018
_diffrn_reflns_theta_max         29.018
_diffrn_reflns_theta_min         3.018
_exptl_absorpt_coefficient_mu    1.911
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.25
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.480
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          1.000
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.60
_refine_diff_density_min         -0.67
_refine_ls_abs_structure_details 'Flack (1983), 1890 Friedel-pairs'
_refine_ls_abs_structure_Flack   -0.015(7)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9978
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         4479
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0430
_refine_ls_R_factor_gt           0.0336
_refine_ls_shift/su_max          0.0012353
_refine_ls_shift/su_mean         0.0000343
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
Method= Modified Sheldrick
w=1/[\s^2^(F^2^) + ( 0.03P)^2^ + 2.95P], where P=(max(Fo^2^,0) + 2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0733
_refine_ls_wR_factor_gt          0.0661
_refine_ls_wR_factor_ref         0.0733
_reflns_number_gt                3882
_reflns_number_total             4493
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            eg3048.cif
_cod_data_source_block           II
_cod_original_sg_symbol_H-M      'P 21 21 21 '
_cod_original_formula_sum        'C23 H26 Br1 N3 O4'
_cod_database_code               2017662