An unexpected co-crystal with a variable degree of order: 1:1 <i>rac</i>-1,2-cyclohexanediol/triphenylphosphine oxide
Siegler, Maxime A.; Fu, Yigang; Simpson, Greg H.; King, Daniel P.; Parkin, Sean; Brock, Carolyn Pratt; Acta Crystallographica Section B 63 (2007) 912–925; doi:10.1107/S0108768107054699

data_2103025
_publ_section_title
;
 An unexpected co-crystal with a variable degree of order: 1:1
 <i>rac</i>-1,2-cyclohexanediol/triphenylphosphine oxide
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              912
_journal_page_last               925
_journal_paper_doi               10.1107/S0108768107054699
_journal_volume                  63
_journal_year                    2007
_chemical_formula_moiety         'C6 H12 O2, C18 H15 O P'
_chemical_formula_sum            'C24 H27 O3 P'
_chemical_formula_weight         394.43
_chemical_name_systematic
;
1:1 rac-1,2-cyclohexanediol triphenylphosphine oxide
;
_space_group_IT_number           2
_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 and CPBrock'
_cell_angle_alpha                100.770(10)
_cell_angle_beta                 102.530(10)
_cell_angle_gamma                90.020(10)
_cell_formula_units_Z            4
_cell_length_a                   9.2710(10)
_cell_length_b                   10.9230(10)
_cell_length_c                   21.306(2)
_cell_measurement_reflns_used    7792
_cell_measurement_temperature    90.0(2)
_cell_measurement_theta_max      67.79
_cell_measurement_theta_min      2.16
_cell_volume                     2067.2(4)
_computing_cell_refinement       'Saintplus in APEX2 (Bruker-Nonius,2004)'
_computing_data_collection       'APEX2 (Bruker-Nonius, 2004)'
_computing_data_reduction        'Saintplus in APEX2 (Bruker-Nonius,2004)'
_computing_molecular_graphics    'Mercury (Macrae et al., 2006)'
_computing_publication_material
;
SHELXL-97 (Sheldrick, 1997) and local procedures
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
;
MULTAN (Main et al., 1977) and DIRDIF (Beurskens, et al., 1983)
;
_diffrn_ambient_temperature      90.0(2)
_diffrn_detector_area_resol_mean 18
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Bruker-Nonius X8 Proteum'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'graded multi-layer optics'
_diffrn_radiation_source         'fine-focus rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0549
_diffrn_reflns_av_sigmaI/netI    0.0546
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            28054
_diffrn_reflns_theta_full        68.17
_diffrn_reflns_theta_max         68.17
_diffrn_reflns_theta_min         2.16
_diffrn_standards_interval_count <1.
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.348
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.77
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS in APEX2 (Bruker-Nonius, 2004)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.267
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lath
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.290
_refine_diff_density_min         -0.422
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     564
_refine_ls_number_reflns         7346
_refine_ls_number_restraints     148
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0479
_refine_ls_R_factor_gt           0.0388
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0363P)^2^+0.8227P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0928
_refine_ls_wR_factor_ref         0.0980
_reflns_number_gt                6312
_reflns_number_total             7346
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            de5032.cif
_cod_data_source_block           toluene90KtriCuKa
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               2103025
_cod_database_fobs_code          2103025