Synthesis, Structure and Cation-Binding Properties of Some [4 + 4] Metallocyclic MO2(2+) (M = Mo or W) Derivatives of 9-Phenyl-2,3,7-trihydroxyfluor-6-one.
McCormick, Laura J.; Abrahams, Brendan F.; Boughton, Berin A.; Grannas, Martin J.; Hudson, Timothy A.; Robson, Richard; Inorganic chemistry 53 (2014) 1721–1728; doi:10.1021/ic402860r

data_4337414
_publ_section_title
;
 Synthesis, Structure and Cation-Binding Properties of Some [4 + 4]
 Metallocyclic MO2(2+) (M = Mo or W) Derivatives of
 9-Phenyl-2,3,7-trihydroxyfluor-6-one.
;
_journal_issue                   3
_journal_name_full               'Inorganic chemistry'
_journal_page_first              1721
_journal_page_last               1728
_journal_paper_doi               10.1021/ic402860r
_journal_volume                  53
_journal_year                    2014
_chemical_formula_sum            'C155 H151 Mo4 N O34.5 P3'
_chemical_formula_weight         3056.44
_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                73.209(2)
_cell_angle_beta                 82.452(2)
_cell_angle_gamma                87.043(2)
_cell_formula_units_Z            2
_cell_length_a                   14.7748(3)
_cell_length_b                   21.8810(5)
_cell_length_c                   24.4420(5)
_cell_measurement_reflns_used    25799
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      73.4432
_cell_measurement_theta_min      3.0171
_cell_volume                     7498.6(3)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      130(2)
_diffrn_detector_area_resol_mean 16.0711
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0310
_diffrn_reflns_av_sigmaI/netI    0.0501
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            74331
_diffrn_reflns_theta_full        70.00
_diffrn_reflns_theta_max         70.00
_diffrn_reflns_theta_min         3.02
_exptl_absorpt_coefficient_mu    3.594
_exptl_absorpt_correction_T_max  0.695
_exptl_absorpt_correction_T_min  0.375
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
Numerical absorption correction based on gaussian integration over a 
multifaceted crystal model
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.354
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3154
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.11
_platon_squeeze_details
;
Solvent accessible voids of ~572 A^3 containing highly disordered 
solvent molecules were found within in the structure. Attempts to 
model the remaining electron density as solvent molecules proved 
unsuccessful. The PLATON/SQUEEZE routine was performed which found 
60 electrons per unit cell. This corresponds to 3 MeOH molecules 
per unit cell which were included in the formula.
;
_refine_diff_density_max         2.640
_refine_diff_density_min         -1.894
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1986
_refine_ls_number_reflns         28126
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0949
_refine_ls_R_factor_gt           0.0712
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1525P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2253
_refine_ls_wR_factor_ref         0.2413
_reflns_number_gt                17835
_reflns_number_total             28126
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic402860r_si_002.cif
_cod_data_source_block           1_Mo3MePPh3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C155 H151 Mo4 N O34.50 P3'
_cod_database_code               4337414