Molybdocalixarene Structure Control via Rim Deprotonation. Synthesis, Characterization, and Crystal Structures of Calix[4]arene Mo(VI) Monooxo Complexes and Calix[4]arene Alkali Metal/Mo(VI) Dioxo Complexes
Liu, Lihua; Zakharov, Lev N.; Golen, James A.; Rheingold, Arnold L.; Watson, William H.; Hanna, Tracy A.; Inorganic Chemistry 45 (2006) 4247–4260; doi:10.1021/ic060404d

data_4332456
_publ_section_title
;
 Molybdocalixarene Structure Control via Rim Deprotonation. Synthesis,
 Characterization, and Crystal Structures of Calix[4]arene Mo(VI) Monooxo
 Complexes and Calix[4]arene Alkali Metal/Mo(VI) Dioxo Complexes
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_journal_issue                   10
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4247
_journal_page_last               4260
_journal_paper_doi               10.1021/ic060404d
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C142 H131 K8 Mo4 N4 O25'
_chemical_formula_weight         3142.51
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.314(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   32.783(3)
_cell_length_b                   32.918(3)
_cell_length_c                   29.183(2)
_cell_measurement_reflns_used    7178
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.20
_cell_measurement_theta_min      2.24
_cell_volume                     30881(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0970
_diffrn_reflns_av_sigmaI/netI    0.1251
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            72734
_diffrn_reflns_theta_full        24.00
_diffrn_reflns_theta_max         24.00
_diffrn_reflns_theta_min         1.06
_exptl_absorpt_coefficient_mu    0.602
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.731
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Dark
_exptl_crystal_density_diffrn    1.353
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             12864
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.612
_refine_diff_density_min         -0.849
_refine_diff_density_rms         0.220
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1580
_refine_ls_number_reflns         24269
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.1536
_refine_ls_R_factor_gt           0.0727
_refine_ls_shift/su_max          0.053
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1296P)^2^+155.8729P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1991
_refine_ls_wR_factor_ref         0.2608
_reflns_number_gt                13017
_reflns_number_total             24269
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060404dsup1.cif
_cod_data_source_block           tcu28
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        30880(4)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4332456