Bi-, Tri-, and Tetranuclear Metallomacrocycles Constructed by Metal-Directed Reactions Involving Resorcinol or Hydroquinone or by Addition of Octahedral Metal Centers to Tetrahexylcalix[4]resorcinarene: X-ray Crystal Structure of syn,syn-[Mo{HB(3,5-Me2C3HN2)3}(NO)(1,4-O2C6H4)]3
Ferida S. McQuillan; Timothy E. Berridge; Hongli Chen; Thomas A. Hamor; Christopher J. Jones; Inorganic Chemistry 37 (1998) 4959–4970; doi:10.1021/ic9803659

data_4323024
_publ_section_title
;
 Bi-, Tri-, and Tetranuclear Metallomacrocycles Constructed by
 Metal-Directed Reactions Involving Resorcinol or Hydroquinone or by
 Addition of Octahedral Metal Centers to Tetrahexylcalix[4]resorcinarene:
 X-ray Crystal Structure of
 syn,syn-[Mo{HB(3,5-Me2C3HN2)3}(NO)(1,4-O2C6H4)]3
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4959
_journal_page_last               4970
_journal_paper_doi               10.1021/ic9803659
_journal_volume                  37
_journal_year                    1998
_chemical_formula_sum            'C63 H78 B3 Mo3 N21 O9'
_chemical_formula_weight         1593.71
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 97.59(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.269(10)
_cell_length_b                   35.310(30)
_cell_length_c                   16.056(10)
_cell_measurement_reflns_used    20568
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      19.4
_cell_measurement_theta_min      1.4
_cell_volume                     9143(11)
_computing_cell_refinement
;
 Unit cell dimensions by post refinement of the full data set
;
_computing_molecular_graphics    ORTEP
_computing_structure_refinement  SHELXL-93
_computing_structure_solution    TEXSAN
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Rigaku area detector diffractometer'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoKa
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0899
_diffrn_reflns_av_sigmaI/netI    0.1045
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            '20568 all data with I > 1sigma(I)'
_diffrn_reflns_theta_max         19.41
_diffrn_reflns_theta_min         1.39
_exptl_absorpt_coefficient_mu    0.459
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.158
_exptl_crystal_F_000             3264
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.768
_refine_diff_density_min         -0.348
_refine_diff_density_rms         0.102
_refine_ls_extinction_coef       0.0013(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^l^3^/sin(2q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.017
_refine_ls_goodness_of_fit_obs   1.139
_refine_ls_matrix_type           full
_refine_ls_number_parameters     893
_refine_ls_number_reflns         7490
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_restrained_S_obs      1.139
_refine_ls_R_factor_all          '0.1189 I > 1sigma(I)'
_refine_ls_R_factor_obs          '0.0743 I > 2sigma(I)'
_refine_ls_shift/esd_max         0.004
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[s^2^(Fo^2^)+( 0.1270P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         '0.2307 I > 1sigma(I)'
_refine_ls_wR_factor_obs         '0.1978 I > 2sigma(I)'
_reflns_number_observed          4638
_reflns_number_total             '7490  I > 1sigma(I)'
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9803659.cif
_cod_data_source_block           ferida25mult
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w=1/[s^2^(Fo^2^)+(
0.1270P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was changed to 'calc'.
New tag '_refine_ls_weighting_details' was created. The value of the
new tag was set to 'w=1/[s^2^(Fo^2^)+( 0.1270P)^2^+0.0000P] where
P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        9142.7(112)
_cod_database_code               4323024