Group 6 Metallocalixarenes Bearing "Hydrazido(2-)" Groups
Carl Redshaw; Mark R. J. Elsegood; Inorganic Chemistry 39 (2000) 5164–5168; doi:10.1021/ic000098i

data_4321494
_publ_section_title
;
 Group 6 Metallocalixarenes Bearing "Hydrazido(2-)" Groups
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5164
_journal_page_last               5168
_journal_paper_doi               10.1021/ic000098i
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C62 H71 N5 O4 W'
_chemical_formula_weight         1134.09
_chemical_name_systematic
;
 ?
;
_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
_cell_angle_alpha                94.057(2)
_cell_angle_beta                 91.513(2)
_cell_angle_gamma                108.029(2)
_cell_formula_units_Z            2
_cell_length_a                   10.7852(6)
_cell_length_b                   14.7376(8)
_cell_length_c                   18.2479(9)
_cell_measurement_reflns_used    14244
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      28.38
_cell_measurement_theta_min      2.23
_cell_volume                     2747.6(3)
_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 0.974
_diffrn_measured_fraction_theta_max 0.857
_diffrn_measurement_device_type  'Bruker SMART CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_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  0.0234
_diffrn_reflns_av_sigmaI/netI    0.0228
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            16884
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.36
_diffrn_reflns_theta_min         1.76
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.154
_exptl_absorpt_correction_T_max  0.661
_exptl_absorpt_correction_T_min  0.406
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.371
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.852
_refine_diff_density_min         -1.045
_refine_diff_density_rms         0.073
_refine_ls_extinction_coef       0.00080(12)
_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   1.064
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     698
_refine_ls_number_reflns         11800
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0256
_refine_ls_R_factor_gt           0.0227
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0284P)^2^+2.6383P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0554
_refine_ls_wR_factor_ref         0.0576
_reflns_number_gt                11128
_reflns_number_total             11800
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic000098i_1.cif
_cod_data_source_block           1
_cod_database_code               4321494