Synthesis and Characterization of Aluminum- and Gallium-Bridged [1.1]Chromarenophanes and [1.1]Molybdarenophanes
Clinton L. Lund; Jörg A. Schachner; Ian J. Burgess; J. Wilson Quail; Gabriele Schatte; Inorganic Chemistry 47 (2008) 5992–6000; doi:10.1021/ic800336f

data_4305359
_publ_contact_author_address
; Department of Chemistry
  University of Saskatchewan
  Saskatoon, Saskatchewan S7N 5C9
  Canada
;
_publ_contact_author_email       jens.mueller@usask.ca
_publ_contact_author_fax         '001 306 966 4730'
_publ_contact_author_name        'Dr Jens Mueller'
_publ_contact_author_phone       '001 306 966 2466'
_publ_section_title
;
Synthesis and Characterization of Aluminum- and Gallium-Bridged
[1.1]Chromarenophanes and [1.1]Molybdarenophanes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5992
_journal_page_last               6000
_journal_paper_doi               10.1021/ic800336f
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C50 H60 Al2 Cr2 N2, 2(C6 H6)'
_chemical_formula_sum            'C62 H72 Al2 Cr2 N2'
_chemical_formula_weight         1003.18
_chemical_name_systematic
; 
 ? 
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 100.756(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.9626(9)
_cell_length_b                   19.3350(18)
_cell_length_c                   12.4626(9)
_cell_measurement_reflns_used    4453
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      0.998
_cell_volume                     2595.2(4)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1998)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_method       '\f scans and \w scans with \k offsets'
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0979
_diffrn_reflns_av_sigmaI/netI    0.1174
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8155
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         3.46
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.494
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.284
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       chip
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.278
_refine_diff_density_min         -0.304
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     294
_refine_ls_number_reflns         4567
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.1317
_refine_ls_R_factor_gt           0.0653
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0420P)^2^+1.6999P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1212
_refine_ls_wR_factor_ref         0.1452
_reflns_number_gt                2686
_reflns_number_total             4567
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic800336f-file002_3.cif
_cod_data_source_block           4a
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4305359