(<i>S</i>)-4,16-Dihydroxymethyl-[2.2]paracyclophane bis-(1<i>S</i>)-camphanoate
Jones, Peter G.; Hillmer, Jörg; Hopf, Henning; Acta Crystallographica Section E 59 (2003) o24–o25; doi:10.1107/S1600536802022328

data_2201775
_publ_section_title
;
 (<i>S</i>)-4,16-Dihydroxymethyl-[2.2]paracyclophane
 bis-(1<i>S</i>)-camphanoate
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o24
_journal_page_last               o25
_journal_paper_doi               10.1107/S1600536802022328
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          'C38 H44 O8'
_chemical_formula_moiety         'C38 H44 O8'
_chemical_formula_sum            'C38 H44 O8'
_chemical_formula_weight         628.73
_chemical_name_systematic
;
 (S)-4,16-Dihydroxymethyl-[2.2]paracyclophane bis-(1S)-camphanoate
;
_space_group_IT_number           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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                67.18(2)
_cell_angle_beta                 81.59(2)
_cell_angle_gamma                85.49(2)
_cell_formula_units_Z            1
_cell_length_a                   6.740(2)
_cell_length_b                   11.295(3)
_cell_length_c                   11.647(3)
_cell_measurement_reflns_used    49
_cell_measurement_temperature    178(2)
_cell_measurement_theta_max      11.5
_cell_measurement_theta_min      10
_cell_volume                     808.2(4)
_computing_cell_refinement       P3
_computing_data_collection       'P3 (Nicolet, 1987)'
_computing_data_reduction        'XDISK (1987)'
_computing_molecular_graphics    'XP (Siemens, 1994)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      178(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Nicolet R3'
_diffrn_measurement_method       \wn
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_sigmaI/netI    0.0270
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            4034
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         3.06
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 147
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.090
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.292
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             336
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.191
_refine_diff_density_min         -0.220
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     421
_refine_ls_number_reflns         4034
_refine_ls_number_restraints     453
_refine_ls_restrained_S_all      0.979
_refine_ls_R_factor_all          0.0467
_refine_ls_R_factor_gt           0.0366
_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^)+(0.0482P)^2^+0.1873P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0876
_refine_ls_wR_factor_ref         0.0949
_reflns_number_gt                3519
_reflns_number_total             4034
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bt6213.cif
_cod_data_source_block           3
_cod_database_code               2201775
_cod_database_fobs_code          2201775