Monometalated tribenzotriquinacene: exo and endo coordination of sodium and potassium with a rigid bowl-shaped hydrocarbon anion
Jan Klett; Chem.Commun. 50 (2014) 7929–; doi:10.1039/C4CC01428F

data_7115285
_publ_section_title
;
 Monometalated tribenzotriquinacene: exo and endo coordination of sodium
 and potassium with a rigid bowl-shaped hydrocarbon anion
;
_journal_name_full               Chem.Commun.
_journal_page_first              7929
_journal_paper_doi               10.1039/C4CC01428F
_journal_volume                  50
_journal_year                    2014
_chemical_formula_sum            'C37 H45 K O3'
_chemical_formula_weight         576.83
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 102.75(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.783(2)
_cell_length_b                   12.416(2)
_cell_length_c                   15.368(2)
_cell_measurement_reflns_used    9887
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      69.283
_cell_measurement_theta_min      4.468
_cell_volume                     3123.4(8)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Bruker SMART 6000 diffractometer '
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54188
_diffrn_reflns_av_R_equivalents  0.0196
_diffrn_reflns_av_unetI/netI     0.0345
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            27313
_diffrn_reflns_point_group_measured_fraction_full 0.807
_diffrn_reflns_point_group_measured_fraction_max 0.797
_diffrn_reflns_theta_full        67.688
_diffrn_reflns_theta_max         69.460
_diffrn_reflns_theta_min         4.470
_diffrn_source                   'rotating anode'
_exptl_absorpt_coefficient_mu    1.750
_exptl_absorpt_correction_T_max  0.7532
_exptl_absorpt_correction_T_min  0.5898
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2012/1
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.227
_exptl_crystal_description       plate
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.163
_refine_diff_density_min         -0.093
_refine_diff_density_rms         0.026
_refine_ls_abs_structure_details
;
 Flack x determined using 1788 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.044(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         4682
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0202
_refine_ls_R_factor_gt           0.0201
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0159P)^2^+0.8710P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0485
_refine_ls_wR_factor_ref         0.0486
_reflns_Friedel_coverage         0.639
_reflns_Friedel_fraction_full    0.635
_reflns_Friedel_fraction_max     0.622
_reflns_number_gt                4649
_reflns_number_total             4682
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4cc01428f2_all.cif
_cod_data_source_block           Go7
_cod_database_code               7115285
_shelx_estimated_absorpt_t_min   0.844
_shelx_estimated_absorpt_t_max   0.949
_shelxl_version_number           2013-4
_shelx_res_checksum              89630