A novel ligand family based on bulky metallocalix[4 and 8]arene substituents
Gibson, Vernon C.; Redshaw, Carl; Elsegood, Mark R. J.; New Journal of Chemistry 26 (2002) 16–19; doi:10.1039/b108088c

data_7052474
_publ_section_title
;
 A novel ligand family based on bulky metallocalix[4 and 8]arene
 substituents
;
_journal_issue                   1
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              16
_journal_page_last               19
_journal_paper_doi               10.1039/b108088c
_journal_volume                  26
_journal_year                    2002
_chemical_formula_sum            'C156 H187 Mo2 N9 O10'
_chemical_formula_weight         2540.03
_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 except H9 coords freely refined'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 107.908(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.3956(17)
_cell_length_b                   31.216(2)
_cell_length_c                   21.2594(15)
_cell_measurement_reflns_used    44542
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      29.17
_cell_measurement_theta_min      2.57
_cell_volume                     14773.9(18)
_computing_cell_refinement       'local programs'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'SHELXTL and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker SMART 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     0.68780
_diffrn_reflns_av_R_equivalents  0.0786
_diffrn_reflns_av_sigmaI/netI    0.1016
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            83968
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.59
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.228
_exptl_absorpt_correction_T_max  0.989
_exptl_absorpt_correction_T_min  0.952
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.142
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             5400
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.808
_refine_diff_density_min         -1.655
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.953
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1741
_refine_ls_number_reflns         31474
_refine_ls_number_restraints     382
_refine_ls_restrained_S_all      0.952
_refine_ls_R_factor_all          0.1227
_refine_ls_R_factor_gt           0.0670
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1030P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1624
_refine_ls_wR_factor_ref         0.1869
_reflns_number_gt                18014
_reflns_number_total             31474
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b108088c.txt
_cod_data_source_block           3
_cod_original_cell_volume        14773.7(18)
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7052474