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_4332459
_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            'C55 H70.5 Li2 Mo N3.5 O7'
_chemical_formula_weight         1002.47
_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                89.568(2)
_cell_angle_beta                 71.825(2)
_cell_angle_gamma                67.398(2)
_cell_formula_units_Z            2
_cell_length_a                   12.3203(15)
_cell_length_b                   13.7772(17)
_cell_length_c                   17.857(2)
_cell_measurement_temperature    150(2)
_cell_volume                     2636.7(5)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.877
_diffrn_measured_fraction_theta_max 0.877
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w 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  0.0201
_diffrn_reflns_av_sigmaI/netI    0.0506
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            16555
_diffrn_reflns_theta_full        28.36
_diffrn_reflns_theta_max         28.36
_diffrn_reflns_theta_min         1.21
_exptl_absorpt_coefficient_mu    0.302
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.846
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.263
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1058
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.876
_refine_diff_density_min         -0.769
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     669
_refine_ls_number_reflns         11566
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0620
_refine_ls_R_factor_gt           0.0508
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1099P)^2^+1.1381P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1527
_refine_ls_wR_factor_ref         0.1668
_reflns_number_gt                9849
_reflns_number_total             11566
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060404dsup1.cif
_cod_data_source_block           tcu50
_cod_depositor_comments
;
The following automatic conversions were performed:

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

'_exptl_absorpt_correction_type' value 'Multi-scan'
changed to 'multi-scan' 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        2636.8(6)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C55 H70.50 Li2 Mo N3.50 O7'
_cod_database_code               4332459