Polymorphism and Solid-Solid Phase Transitions of Hydrogen Bonded 2-adamantanol and 2-methyl-2-adamantanol Compounds
Salvatori, Alejandro; Négrier, Philippe; Massip, Stephane; Munoz-Duque, Antoni; Lloveras, Pol; Barrio, Maria; Tamarit, Josep Lluis; CrystEngComm  (2022) –; doi:10.1039/D2CE00324D

data_7244791
_publ_section_title
;
 Polymorphism and Solid-Solid Phase Transitions of Hydrogen Bonded
 2-adamantanol and 2-methyl-2-adamantanol Compounds
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE00324D
_journal_year                    2022
_chemical_formula_moiety         'C10 H16 O'
_chemical_formula_sum            'C10 H16 O'
_chemical_formula_weight         152.23
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2021-12-17 deposited with the CCDC.	2022-04-14 downloaded from the CCDC.
;
_cell_angle_alpha                82.116(3)
_cell_angle_beta                 70.323(3)
_cell_angle_gamma                62.123(4)
_cell_formula_units_Z            6
_cell_length_a                   11.4076(4)
_cell_length_b                   11.4418(5)
_cell_length_c                   11.4575(4)
_cell_measurement_reflns_used    14621
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      75.6160
_cell_measurement_theta_min      4.0410
_cell_volume                     1244.37(10)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43'
_computing_data_collection       'CrystalClear-SM Expert 2.1 (Rigaku, 2013)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Superflip 03/15/13 12:43'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 PILT
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device       'AFC11 (Right): Eulerian 3 circle'
_diffrn_measurement_device_type  'Rigaku PILATUS conversion'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0288
_diffrn_reflns_av_unetI/netI     0.0172
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            16978
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.112
_diffrn_reflns_theta_min         4.099
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    0.585
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45590
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.219
_exptl_crystal_description       prism
_exptl_crystal_F_000             504
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.173
_refine_diff_density_min         -0.347
_refine_diff_density_rms         0.066
_refine_ls_extinction_coef       0.0241(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014)'
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     311
_refine_ls_number_reflns         4832
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_gt           0.0465
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0773P)^2^+0.3081P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1334
_refine_ls_wR_factor_ref         0.1359
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4420
_reflns_number_total             4832
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00324d2.cif
_cod_data_source_block           ada2oh150K
_cod_original_cell_volume        1244.37(9)
_cod_database_code               7244791
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.868
_shelx_estimated_absorpt_t_max   0.917
_shelx_res_checksum              24525
_shelx_hkl_checksum              17549