Crystal Structures and Glassy Phase Transition Behavior of Cyclohexene
Ibberson, Richard M.; Telling, Mark T. F.; Parsons, Simon; Crystal Growth & Design 8 (2008) 512–; doi:10.1021/cg0705512

data_4503126
_publ_section_title
;
 Crystal Structures and Glassy Phase Transition Behavior of Cyclohexene
;
_journal_issue                   2
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              512
_journal_paper_doi               10.1021/cg0705512
_journal_volume                  8
_journal_year                    2008
_chemical_compound_source        'Aldrich '
_chemical_formula_moiety         'C6 H10'
_chemical_formula_sum            'C6 H10'
_chemical_formula_weight         82.14
_chemical_melting_point          170
_chemical_name_systematic
; 
Cyclohexene-III
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             06-11-18
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.673(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   10.699(7)
_cell_length_b                   10.232(7)
_cell_length_c                   9.759(7)
_cell_measurement_reflns_used    1000
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      21.5
_cell_measurement_theta_min      2.5
_cell_volume                     1068.3(13)
_computing_cell_refinement       Saint
_computing_data_collection       Smart
_computing_data_reduction        Saint
_computing_molecular_graphics    XP
_computing_publication_material  'XCIF, PLATON'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       omega
_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  0.0468
_diffrn_reflns_av_sigmaI/netI    0.0440
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            4911
_diffrn_reflns_theta_full        22.49
_diffrn_reflns_theta_max         22.49
_diffrn_reflns_theta_min         1.90
_exptl_absorpt_coefficient_mu    0.057
_exptl_absorpt_correction_T_max  0.976
_exptl_absorpt_correction_T_min  0.483
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs scaled by 1.31'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.025
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cylinder
_exptl_crystal_F_000             368
_exptl_crystal_recrystallization_method
;
OHCD Laser-assisted crystal growth:
Max voltage: 2V
Temperature of growth 160K
Program:

Start Position  End Position  Start Power  End powder  Time
--------------------------------------------------------------
    88%             60%           70%        70%       20 min
    60%             60%           70%         0%        5 min

Cell after growth: cubic P a = 10.35 (phase I)

Then ramp at 360 K/hr to 110 K

Cell metrically orthorhombic, but solution indicates monoclinic 
symmetry.

;
_exptl_crystal_size_max          3.20
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.44
_refine_diff_density_max         0.165
_refine_diff_density_min         -0.144
_refine_diff_density_rms         0.034
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     129
_refine_ls_number_reflns         1386
_refine_ls_number_restraints     285
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0615
_refine_ls_R_factor_gt           0.0472
_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^)+(0.0723P)^2^+0.0918P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1172
_refine_ls_wR_factor_ref         0.1261
_reflns_number_gt                1148
_reflns_number_total             1386
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg0705512-file002.cif
_cod_data_source_block           ri6001
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Multiscan'
changed to 'multi-scan' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        1064.0(13)
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4503126