3,3,3',3'-Tetramethyl-6,6'-bis[(pyridin-4-yl)methoxy]-1,1'-spirobiindane monohydrate
Zhang, Ya-Jie; Sun, Yan; Gao, Shu-Mei; Jiang, Xiao-Qing; Deng, Yu-Heng; Acta Crystallographica Section E 68 (2012) o1763–o1764; doi:10.1107/S1600536812021289

data_2235008
_publ_section_title
;
 3,3,3',3'-Tetramethyl-6,6'-bis[(pyridin-4-yl)methoxy]-1,1'-spirobiindane
 monohydrate
;
_journal_coeditor_code           GO2055
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1763
_journal_page_last               o1764
_journal_paper_doi               10.1107/S1600536812021289
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C33 H34 N2 O2, H2 O'
_chemical_formula_moiety         'C33 H34 N2 O2, H2 O'
_chemical_formula_sum            'C33 H36 N2 O3'
_chemical_formula_weight         508.64
_chemical_name_systematic
;
3,3,3',3'-Tetramethyl-6,6'-bis[(pyridin-4-yl)methoxy]-1,1'-spirobiindane
monohydrate
;
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_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
_cell_angle_alpha                81.92(3)
_cell_angle_beta                 87.17(3)
_cell_angle_gamma                77.22(3)
_cell_formula_units_Z            2
_cell_length_a                   6.0101(12)
_cell_length_b                   10.724(2)
_cell_length_c                   22.156(4)
_cell_measurement_reflns_used    3702
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.3435
_cell_measurement_theta_min      1.8571
_cell_volume                     1378.6(5)
_computing_cell_refinement       '<i>APEX2</i> and <i>SAINT</i> (Bruker, 2007)'
_computing_data_collection       '<i>APEX2</i> (Bruker, 2007)'
_computing_data_reduction        '<i>APEX2</i> and <i>SAINT</i> (Bruker, 2007)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2001)'
_computing_publication_material  '<i>SHELXTL</i> (Sheldrick, 2008)'
_computing_structure_refinement  '<i>SHELXL97</i> (Sheldrick, 2008)'
_computing_structure_solution    '<i>SHELXS97</i> (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \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  0.0337
_diffrn_reflns_av_sigmaI/netI    0.0445
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            10554
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.34
_diffrn_reflns_theta_min         2.88
_exptl_absorpt_coefficient_mu    0.078
_exptl_absorpt_correction_T_max  0.9838
_exptl_absorpt_correction_T_min  0.9627
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(<i>SADABS</i>; Bruker, 2007)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.225
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             544
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.237
_refine_diff_density_min         -0.173
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.156
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     347
_refine_ls_number_reflns         4988
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.156
_refine_ls_R_factor_all          0.0826
_refine_ls_R_factor_gt           0.0685
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0350P)^2^+0.7601P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1302
_refine_ls_wR_factor_ref         0.1372
_reflns_number_gt                4253
_reflns_number_total             4988
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            go2055.cif
_cod_data_source_block           I
_cod_database_code               2235008
_cod_database_fobs_code          2235008