New <i>C</i>2-symmetric cyclopentadiene dimer from sodium naphthalenide reduction of 1,3,6-tri-<i>tert</i>-butylfulvene
Bragg, Sarah; Johnson, Jane E.B.; Graziano, Gina M.; Balaich, Gary J.; Heimer, Norman E.; Acta Crystallographica Section E 58 (2002) o1010–o1012; doi:10.1107/S1600536802013089

data_2201608
_publ_section_title
;
 New <i>C</i>2-symmetric cyclopentadiene dimer from sodium
 naphthalenide reduction of 1,3,6-tri-<i>tert</i>-butylfulvene
;
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1010
_journal_page_last               o1012
_journal_paper_doi               10.1107/S1600536802013089
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac          'C36 H62'
_chemical_formula_moiety         'C36 H62'
_chemical_formula_sum            'C36 H62'
_chemical_formula_weight         494.886
_chemical_melting_point          160.1
_chemical_name_common
'rac-1,2-bis(1,4-di-tertbutylcyclopentadiene)-1,2-di-tertbutylethane dimer'
_chemical_name_systematic
;
rac-3,4-bis(1,4-di-tertbutylcyclopenta-1,3-dien-2-yl)-2,2,5,5-tetramethyl-
hexane
;
_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_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.9350(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.2790(10)
_cell_length_b                   10.5194(8)
_cell_length_c                   19.680(2)
_cell_measurement_reflns_used    4491
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      22.62
_cell_measurement_theta_min      2.30
_cell_volume                     3345.5(5)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2001)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Bruker, 2001)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.952
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_device_type  'Bruker CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_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    0.0504
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_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            28797
_diffrn_reflns_theta_full        28.39
_diffrn_reflns_theta_max         28.39
_diffrn_reflns_theta_min         2.08
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.054
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.84
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2001)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    0.983
_exptl_crystal_density_meas      0.974
_exptl_crystal_density_method    'correction from room temp data'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.292
_refine_diff_density_min         -0.174
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         7984
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0917
_refine_ls_R_factor_gt           0.0596
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0727P)^2^+0.6485P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1412
_refine_ls_wR_factor_ref         0.1580
_reflns_number_gt                5492
_reflns_number_total             7984
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om6099.cif
_cod_data_source_block           II
_cod_original_cell_volume        3345.4(5)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2201608
_cod_database_fobs_code          2201608