(1<i>R</i>,3<i>S</i>)-Camphoric acid as a building block in supramolecular chemistry: adducts with organic polyamines
Zakaria, Choudhury M.; Ferguson, George; Lough, Alan J.; Glidewell, Christopher; Acta Crystallographica Section B 59 (2003) 118–131; doi:10.1107/S0108768102022358

data_2103845
_publ_section_title
;
 (1<i>R</i>,3<i>S</i>)-Camphoric acid as a building block in
 supramolecular chemistry: adducts with organic polyamines
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              118
_journal_page_last               131
_journal_paper_doi               10.1107/S0108768102022358
_journal_volume                  59
_journal_year                    2003
_chemical_formula_moiety         'C12 H12 N2, C10 H16 O4'
_chemical_formula_sum            'C22 H28 N2 O4'
_chemical_formula_weight         384.46
_chemical_name_systematic
;
(1R,3S)-Camphoric acid--1,2-bis(4-pyridyl)ethane (1/1)
;
_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
_cell_angle_alpha                99.8190(8)
_cell_angle_beta                 95.4780(8)
_cell_angle_gamma                90.7870(9)
_cell_formula_units_Z            4
_cell_length_a                   8.5318(2)
_cell_length_b                   10.3775(2)
_cell_length_c                   23.3884(5)
_cell_measurement_reflns_used    9230
_cell_measurement_temperature    150.0(10)
_cell_measurement_theta_max      27.43
_cell_measurement_theta_min      2.64
_cell_volume                     2030.18(8)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'Kappa-CCD server software (Nonius, 1997)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'PLATON (Spek, 2002)'
_computing_publication_material
'SHELXL-97 (Sheldrick, 1997a) and  PRPKAPPA (Ferguson, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997a)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997b)'
_diffrn_ambient_temperature      150.0(10)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  Kappa-CCD
_diffrn_measurement_method       '\f scans, and \w scans with \k offsets'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.064
_diffrn_reflns_av_sigmaI/netI    0.0554
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            34201
_diffrn_reflns_theta_full        27.43
_diffrn_reflns_theta_max         27.43
_diffrn_reflns_theta_min         2.64
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.087
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.258
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             824
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.257
_refine_diff_density_min         -0.199
_refine_ls_extinction_coef       0.032(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1272
_refine_ls_number_reflns         9230
_refine_ls_number_restraints     241
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0724
_refine_ls_R_factor_gt           0.0494
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0763P)^2^+0.2326P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1234
_refine_ls_wR_factor_ref         0.1377
_reflns_number_gt                7063
_reflns_number_total             9230
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            na0144.cif
_cod_data_source_block           III
_cod_original_cell_volume        2030.17(8)
_cod_database_code               2103845
_cod_database_fobs_code          2103845