A carbanion induced ring switching synthesis of spiranes: an unprecedented approach
Maurya, Hardesh K.; Pratap, Ramendra; Kumar, Abhinav; Kumar, Brijesh; Huch, Volker; Tandon, Vishnu K.; Ji Ram, Vishnu; RSC Advances 2 (2012) 9091–; doi:10.1039/c2ra21587j

data_7238723
_publ_section_title
;
 A carbanion induced ring switching synthesis of spiranes: an
 unprecedented approach
;
_journal_issue                   24
_journal_name_full               'RSC Advances'
_journal_page_first              9091
_journal_paper_doi               10.1039/c2ra21587j
_journal_volume                  2
_journal_year                    2012
_chemical_formula_sum            'C53 H48 Br2 N4 O4'
_chemical_formula_weight         964.75
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_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
_cell_angle_alpha                110.363(5)
_cell_angle_beta                 96.456(5)
_cell_angle_gamma                104.041(5)
_cell_formula_units_Z            1
_cell_length_a                   7.883(5)
_cell_length_b                   11.024(5)
_cell_length_c                   14.736(5)
_cell_measurement_reflns_used    2888
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      29.2455
_cell_measurement_theta_min      2.992
_cell_volume                     1137.1(10)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 15.9853
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.847
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_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  0.0334
_diffrn_reflns_av_sigmaI/netI    0.0634
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            10794
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.31
_diffrn_reflns_theta_min         3.00
_exptl_absorpt_coefficient_mu    1.833
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.46684
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.409
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             496
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.250
_refine_diff_density_min         -0.422
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     283
_refine_ls_number_reflns         5276
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.1261
_refine_ls_R_factor_gt           0.0714
_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^)+(0.0990P)^2^+0.5861P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1698
_refine_ls_wR_factor_ref         0.2021
_reflns_number_gt                3141
_reflns_number_total             5276
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ra21587j.txt
_cod_data_source_block           rp-vjr-123b
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7238723