Correlated rotations in benzylfluorene derivatives: structure, conformation, and stereodynamics.
Casarini, Daniele; Lunazzi, Lodovico; Mazzanti, Andrea; The Journal of organic chemistry 73 (2008) 2811–2818; doi:10.1021/jo7026917

data_4029562
_publ_contact_author
;
Dr. Andrea Mazzanti
University of Bologna
Department of Organic Chemistry A.Mangini
Viale Risorgimento 4
40136 Bologna
Italy
;
_publ_section_title
;
 Correlated rotations in benzylfluorene derivatives: structure,
 conformation, and stereodynamics.
;
_journal_issue                   7
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              2811
_journal_page_last               2818
_journal_paper_doi               10.1021/jo7026917
_journal_volume                  73
_journal_year                    2008
_chemical_formula_sum            'C23 H22'
_chemical_formula_weight         298.41
_chemical_melting_point          94
_chemical_name_common            'compound 2'
_chemical_name_systematic
; 
 9-(2,4,6-trimethylbenzyl)-9H-fluorene  
;
_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             19/07/2007
_audit_creation_method           SHELXL-97
_audit_update_record             14/12/2007
_cell_angle_alpha                90.00
_cell_angle_beta                 112.882(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.134(2)
_cell_length_b                   15.891(3)
_cell_length_c                   11.545(2)
_cell_measurement_temperature    273(2)
_cell_volume                     1712.9(6)
_computing_cell_refinement       'Bruker APEX v1.0.27'
_computing_data_collection       'Bruker APEX v1.0.27'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.937
_diffrn_measured_fraction_theta_max 0.937
_diffrn_measurement_device_type  'Bruker APEX 2'
_diffrn_measurement_method       'Phi and omega scans'
_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  0.0306
_diffrn_reflns_av_sigmaI/netI    0.0226
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            19148
_diffrn_reflns_theta_full        28.64
_diffrn_reflns_theta_max         28.64
_diffrn_reflns_theta_min         2.18
_exptl_absorpt_coefficient_mu    0.065
_exptl_absorpt_correction_T_max  0.9745
_exptl_absorpt_correction_T_min  0.9499
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.157
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       brick
_exptl_crystal_F_000             640
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.163
_refine_diff_density_min         -0.179
_refine_diff_density_rms         0.031
_refine_ls_extinction_coef       0.097(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     212
_refine_ls_number_reflns         4127
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0562
_refine_ls_R_factor_gt           0.0451
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0669P)^2^+0.2066P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1247
_refine_ls_wR_factor_ref         0.1349
_reflns_number_gt                3233
_reflns_number_total             4127
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo7026917-file003.cif
_cod_data_source_block           fluorene
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4029562