Calixarenes as ligands for transition-metal catalysts: a bis(calix[4]arene-11,23-dicarboxylato) dirhodium complex
Seitz, Jürgen; Maas, Gerhard; Chemical Communications  (2002) 338–; doi:10.1039/b110478k

data_7114113
_publ_section_title
;
 Calixarenes as ligands for transition-metal catalysts: a
 bis(calix[4]arene-11,23-dicarboxylato) dirhodium complex
;
_journal_issue                   4
_journal_name_full               'Chemical Communications'
_journal_page_first              338
_journal_paper_doi               10.1039/b110478k
_journal_year                    2002
_chemical_formula_moiety         '(C84H88BR4O16RH2) x 4(C7H8)'
_chemical_formula_sum            'C224 H240 B Br4 O32 R4 Rh4'
_chemical_formula_weight         2247.54
_chemical_melting_point          563.15
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method
;SHELXL-97 
bis(5,17-dibromocalix[4]arene-11,23-dicarboxylato) dirhodium toluene 
tetrasolvate
;
_cell_angle_alpha                72.15(2)
_cell_angle_beta                 87.38(2)
_cell_angle_gamma                85.48(2)
_cell_formula_units_Z            2
_cell_length_a                   12.801(2)
_cell_length_b                   16.916(3)
_cell_length_c                   25.080(5)
_cell_measurement_temperature    193(2)
_cell_volume                     5152.0(17)
_computing_cell_refinement       'IPDS software (Stoe, Darmstadt)'
_computing_data_collection       'IPDS software (Stoe, Darmstadt)'
_computing_data_reduction        'X-RED (Stoe, Darmstadt)'
_computing_molecular_graphics    'ORTEP-3 for Windows (L.J. Farrugia, 1998)'
_computing_publication_material  'SHELXL-97 (G. M. Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (G. M. Sheldrick, 1997)'
_computing_structure_solution    SIR-92
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.955
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_device_type  'IPDS (Stoe, Darmstadt)'
_diffrn_measurement_method       'Phi scans, rotation mode'
_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  0.0668
_diffrn_reflns_av_sigmaI/netI    0.1080
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            26124
_diffrn_reflns_theta_full        21.97
_diffrn_reflns_theta_max         21.97
_diffrn_reflns_theta_min         2.11
_exptl_absorpt_coefficient_mu    1.936
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.449
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2300
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.31
_refine_diff_density_max         1.976
_refine_diff_density_min         -0.795
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.950
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1146
_refine_ls_number_reflns         12010
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      0.951
_refine_ls_R_factor_all          0.1037
_refine_ls_R_factor_gt           0.0641
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0946P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1520
_refine_ls_wR_factor_ref         0.1661
_reflns_number_gt                7370
_reflns_number_total             12010
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b110478k.txt
_cod_data_source_block           JSE013
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value ' 290 \%C' was changed to '563.15' -
it was converted from degrees Celsius(C) to Kelvins(K).

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        5151.9(17)
_cod_original_sg_symbol_H-M      'P 1bar'
_cod_original_formula_sum        'C112 H120 Br4 O16 Rh2 C112 H120 BR4 O16 Rh2'
_cod_database_code               7114113