Generation and Reactions of an Octacyclic Hindered Pyramidalized Alkene.
Camps, Pelayo; Lozano, David; Barbaraci, Carla; Font-Bardia, Merce; Luque, F. Javier; Estarellas, Carolina; The Journal of organic chemistry 83 (2018) 5420–5430; doi:10.1021/acs.joc.8b00212

data_4034812
_publ_section_title
;
 Generation and Reactions of an Octacyclic Hindered Pyramidalized Alkene.
;
_journal_issue                   10
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              5420
_journal_page_last               5430
_journal_paper_doi               10.1021/acs.joc.8b00212
_journal_volume                  83
_journal_year                    2018
_chemical_formula_moiety         'C19 H20'
_chemical_formula_sum            'C19 H20'
_chemical_formula_weight         248.35
_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   geom
_audit_creation_method           SHELXL-2012
_cell_angle_alpha                105.046(2)
_cell_angle_beta                 96.566(2)
_cell_angle_gamma                90.113(2)
_cell_formula_units_Z            4
_cell_length_a                   5.9104(4)
_cell_length_b                   11.1856(8)
_cell_length_c                   19.9679(14)
_cell_measurement_reflns_used    9935
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.52
_cell_measurement_theta_min      2.40
_cell_volume                     1265.80(15)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_structure_solution    'XT-2014 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0449
_diffrn_reflns_av_unetI/netI     0.0243
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            71539
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.567
_diffrn_reflns_theta_min         2.447
_diffrn_source                   microfocus
_exptl_absorpt_coefficient_mu    0.073
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6714
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.303
_exptl_crystal_description       prism
_exptl_crystal_F_000             536
_exptl_crystal_size_max          0.440
_exptl_crystal_size_mid          0.103
_exptl_crystal_size_min          0.058
_refine_diff_density_max         0.505
_refine_diff_density_min         -0.338
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         7702
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0651
_refine_ls_R_factor_gt           0.0545
_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^)+(0.0795P)^2^+0.9711P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1622
_refine_ls_wR_factor_ref         0.1700
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6307
_reflns_number_total             7702
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo8b00212_si_004.cif
_cod_data_source_block           mo_D28VB72_0m_a
_cod_database_code               4034812
_shelxl_version_number           2012-9
_shelx_res_checksum              55385
_shelx_hkl_checksum              65918