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

data_4321495
_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            'C120.5 H138 Cl5 N7 O8 W2'
_chemical_formula_weight         2357.33
_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                94.791(6)
_cell_angle_beta                 108.422(5)
_cell_angle_gamma                99.972(8)
_cell_formula_units_Z            2
_cell_length_a                   16.7386(14)
_cell_length_b                   18.809(2)
_cell_length_c                   20.0969(17)
_cell_measurement_reflns_used    551
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      28.5
_cell_measurement_theta_min      2.7
_cell_volume                     5847.2(10)
_computing_cell_refinement       'Bruker SMAR'
_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 0.962
_diffrn_measured_fraction_theta_max 0.925
_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     0.68750
_diffrn_reflns_av_R_equivalents  0.0450
_diffrn_reflns_av_sigmaI/netI    0.0930
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            38641
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.90
_diffrn_standards_decay_%        15
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.136
_exptl_absorpt_correction_T_max  0.9194
_exptl_absorpt_correction_T_min  0.5861
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2414
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         4.491
_refine_diff_density_min         -4.097
_refine_diff_density_rms         0.188
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.986
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1386
_refine_ls_number_reflns         27466
_refine_ls_number_restraints     334
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.0718
_refine_ls_R_factor_gt           0.0554
_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^)+(0.0793P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1444
_refine_ls_wR_factor_ref         0.1511
_reflns_number_gt                20077
_reflns_number_total             27466
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic000098i_2.cif
_cod_data_source_block           2
_cod_original_cell_volume        5847.4(9)
_cod_original_formula_sum        'C120.50 H138 Cl5 N7 O8 W2'
_cod_database_code               4321495