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

data_4321496
_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            'C124 H148 Mo2 N4 O12'
_chemical_formula_weight         2078.34
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.078(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.0888(11)
_cell_length_b                   17.7004(12)
_cell_length_c                   19.4921(14)
_cell_measurement_reflns_used    10923
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      25.70
_cell_measurement_theta_min      2.30
_cell_volume                     5549.9(7)
_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 0.888
_diffrn_measured_fraction_theta_max 0.888
_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  0.0610
_diffrn_reflns_av_sigmaI/netI    0.0589
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            24171
_diffrn_reflns_theta_full        25.87
_diffrn_reflns_theta_max         25.87
_diffrn_reflns_theta_min         1.55
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.288
_exptl_absorpt_correction_T_max  0.955
_exptl_absorpt_correction_T_min  0.924
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'very dark red'
_exptl_crystal_density_diffrn    1.244
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2200
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.826
_refine_diff_density_min         -0.909
_refine_diff_density_rms         0.084
_refine_ls_extinction_coef       0.00089(16)
_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   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     707
_refine_ls_number_reflns         9567
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0845
_refine_ls_R_factor_gt           0.0595
_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^)+(0.0587P)^2^+12.6243P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1362
_refine_ls_wR_factor_ref         0.1520
_reflns_number_gt                7297
_reflns_number_total             9567
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic000098i_3.cif
_cod_data_source_block           3
_cod_database_code               4321496