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_4337420
_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            'C164.5 H194 Mo4 N4 O33.5 P2'
_chemical_formula_weight         3208.94
_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                75.049(2)
_cell_angle_beta                 82.216(2)
_cell_angle_gamma                63.834(2)
_cell_formula_units_Z            2
_cell_length_a                   18.9580(3)
_cell_length_b                   21.1324(6)
_cell_length_c                   22.6782(4)
_cell_measurement_reflns_used    21887
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      73.0198
_cell_measurement_theta_min      4.2104
_cell_volume                     7875.9(3)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.31 (release 08-01-2009 CrysAlis171 .NET)
(compiled Jan  8 2009,16:24:04)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.31 (release 08-01-2009 CrysAlis171 .NET)
(compiled Jan  8 2009,16:24:04)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.31 (release 08-01-2009 CrysAlis171 .NET)
(compiled Jan  8 2009,16:24:04)
;
_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 0.966
_diffrn_measured_fraction_theta_max 0.966
_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  0.0391
_diffrn_reflns_av_sigmaI/netI    0.0678
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            55062
_diffrn_reflns_theta_full        68.00
_diffrn_reflns_theta_max         68.00
_diffrn_reflns_theta_min         4.21
_exptl_absorpt_coefficient_mu    3.351
_exptl_absorpt_correction_T_max  0.794
_exptl_absorpt_correction_T_min  0.369
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.31 (release 08-01-2009 CrysAlis171 .NET)
(compiled Jan  8 2009,16:24:04)
Numerical absorption correction based on gaussian integration 
over a multifaceted crystal model
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.353
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             3350
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.303
_refine_diff_density_min         -1.723
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.966
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     2181
_refine_ls_number_reflns         27709
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.966
_refine_ls_R_factor_all          0.0864
_refine_ls_R_factor_gt           0.0591
_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^)+(0.1043P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1536
_refine_ls_wR_factor_ref         0.1641
_reflns_number_gt                18563
_reflns_number_total             27709
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic402860r_si_002.cif
_cod_data_source_block           7_MoPNP
_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        'C164.50 H194 Mo4 N4 O33.50 P2'
_cod_database_code               4337420