Studies in the rearrangement reactions involving camphorquinone
Rao, H. Surya Prakash; Saha, Ahana; Vijjapu, Satish; RSC Advances 11 (2021) 7180–7186; doi:10.1039/D0RA09839F

data_7242345
_publ_section_title
;
 Studies in the rearrangement reactions involving camphorquinone
;
_journal_issue                   13
_journal_name_full               'RSC Advances'
_journal_page_first              7180
_journal_page_last               7186
_journal_paper_doi               10.1039/D0RA09839F
_journal_volume                  11
_journal_year                    2021
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C13 H21 I O2'
_chemical_formula_sum            'C13 H21 I O2'
_chemical_formula_weight         336.20
_chemical_melting_point          'Not available as it was semi solid'
_chemical_name_common            Nil
_chemical_name_systematic
(2S,3aR,6S,7aR,8S)-2-(iodomethyl)-6,7,7-trimethylhexahydro-2H-3a,6-methanobenzofuran-8-ol
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-12-27 deposited with the CCDC.	2021-01-18 downloaded from the CCDC.
;
_cell_angle_alpha                99.910(2)
_cell_angle_beta                 106.378(2)
_cell_angle_gamma                95.260(2)
_cell_formula_units_Z            4
_cell_length_a                   11.3843(5)
_cell_length_b                   11.4267(5)
_cell_length_c                   11.6597(5)
_cell_measurement_reflns_used    9993
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.98
_cell_measurement_theta_min      2.80
_cell_volume                     1417.63(11)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012), PLATON (Spek, 2020) and
Mercury
(Macrae <i>et al.</i>,  2020)
;
_computing_publication_material
;
ORTEP-3 for Windows (Farrugia, 2012), PLATON (Spek, 2020) and
Mercury
(Macrae <i>et al.</i>,  2020)
;
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0226
_diffrn_reflns_av_unetI/netI     0.0377
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.963
_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       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            19906
_diffrn_reflns_point_group_measured_fraction_full 0.853
_diffrn_reflns_point_group_measured_fraction_max 0.806
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.783
_diffrn_reflns_theta_min         1.829
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.245
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5314
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0799 before and 0.0460 after correction.
The Ratio of minimum to maximum transmission is 0.7129.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear whiteish colourless'
_exptl_crystal_density_diffrn    1.575
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rectangular block'
_exptl_crystal_F_000             672
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.100
_refine_diff_density_max         3.724
_refine_diff_density_min         -0.722
_refine_diff_density_rms         0.130
_refine_ls_abs_structure_details
;
 Flack x determined using 3091 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.046(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     593
_refine_ls_number_reflns         9782
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0650
_refine_ls_R_factor_gt           0.0576
_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^)+(0.1086P)^2^+1.6149P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1656
_refine_ls_wR_factor_ref         0.1725
_reflns_Friedel_coverage         0.674
_reflns_Friedel_fraction_full    0.713
_reflns_Friedel_fraction_max     0.649
_reflns_number_gt                8412
_reflns_number_total             9782
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ra09839f2.cif
_cod_data_source_block           shelx
_cod_database_code               7242345
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.604
_shelx_estimated_absorpt_t_max   0.807
_shelx_res_checksum              12442