New structural motifs in chromium(iii) calix[4 and 6]arene chemistry
Redshaw, Carl; Homden, Damien; Hughes, David L.; Wright, Joseph A.; Elsegood, Mark R. J.; Dalton Transactions  (2009) 1231–1242; doi:10.1039/b813313a

data_7000494
_publ_section_title
;
 New structural motifs in chromium(iii) calix[4 and 6]arene chemistry
;
_journal_issue                   7
_journal_name_full               'Dalton Transactions'
_journal_page_first              1231
_journal_page_last               1242
_journal_paper_doi               10.1039/b813313a
_journal_year                    2009
_chemical_formula_moiety         'C224 H314 Cr4 K6 O34, 6(C4 H8 O)'
_chemical_formula_sum            'C248 H362 Cr4 K6 O40'
_chemical_formula_weight         4425.98
_chemical_name_common            'Compound 3'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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
_cell_angle_alpha                105.255(3)
_cell_angle_beta                 96.182(3)
_cell_angle_gamma                105.001(2)
_cell_formula_units_Z            1
_cell_length_a                   16.9918(18)
_cell_length_b                   17.4045(19)
_cell_length_c                   22.146(2)
_cell_measurement_reflns_used    23903
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      28.62
_cell_measurement_theta_min      2.28
_cell_volume                     5993.6(11)
_computing_cell_refinement       'local programs'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'Bruker SMART 1K CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'Daresbury SRS station 9.8'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6875
_diffrn_reflns_av_R_equivalents  0.0885
_diffrn_reflns_av_sigmaI/netI    0.1870
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            35853
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.80
_diffrn_standards_decay_%        20
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.350
_exptl_absorpt_correction_T_max  0.979
_exptl_absorpt_correction_T_min  0.921
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'semi-empirical from \y-scans'
_exptl_crystal_colour            'colourless/blue dichroic'
_exptl_crystal_density_diffrn    1.226
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2380
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_platon_squeeze_details
;
;
_refine_diff_density_max         3.439
_refine_diff_density_min         -1.147
_refine_diff_density_rms         0.159
_refine_ls_extinction_coef       0.0093(14)
_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   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1427
_refine_ls_number_reflns         22539
_refine_ls_number_restraints     1253
_refine_ls_restrained_S_all      1.248
_refine_ls_R_factor_all          0.1748
_refine_ls_R_factor_gt           0.1261
_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^)+(0.1912P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3240
_refine_ls_wR_factor_ref         0.3470
_reflns_number_gt                11660
_reflns_number_total             22539
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b813313a.txt
_cod_data_source_block           3
_cod_original_cell_volume        5993.7(11)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7000494