Dinuclear Zinc(II) Complexes with Hydrogen Bond Donors as Structural and Functional Phosphatase Models.
Bosch, Simone; Comba, Peter; Gahan, Lawrence R.; Schenk, Gerhard; Inorganic chemistry 53 (2014) 9036–9051; doi:10.1021/ic5009945

data_4340738
_publ_section_title
;
 Dinuclear Zinc(II) Complexes with Hydrogen Bond Donors as Structural and
 Functional Phosphatase Models.
;
_journal_issue                   17
_journal_name_full               'Inorganic chemistry'
_journal_page_first              9036
_journal_page_last               9051
_journal_paper_doi               10.1021/ic5009945
_journal_volume                  53
_journal_year                    2014
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C49 H55 N9 O9 P Zn2, P F6, C H4 O, H2 O '
_chemical_formula_sum            'C50 H61 F6 N9 O11 P2 Zn2'
_chemical_formula_weight         1270.76
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_date             2014-04-22T13:08:17-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 107.817(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.5695(6)
_cell_length_b                   23.3831(8)
_cell_length_c                   17.1987(5)
_cell_measurement_reflns_used    3942
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.928
_cell_measurement_theta_min      3.022
_cell_measurement_wavelength     0.71073
_cell_volume                     5578.2(4)
_computing_cell_refinement
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
        (compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
        (compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
        (compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.0696
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0377134
_diffrn_orient_matrix_UB_12      0.0138575
_diffrn_orient_matrix_UB_13      -0.0107159
_diffrn_orient_matrix_UB_21      -0.0073909
_diffrn_orient_matrix_UB_22      0.0250649
_diffrn_orient_matrix_UB_23      0.0205597
_diffrn_orient_matrix_UB_31      0.0336949
_diffrn_orient_matrix_UB_32      -0.0100152
_diffrn_orient_matrix_UB_33      0.036604
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0664
_diffrn_reflns_av_unetI/netI     0.1094
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            22528
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         25
_diffrn_reflns_theta_min         2.89
_exptl_absorpt_coefficient_mu    1.004
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.98414
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
        (compiled Feb  1 2013,16:14:44)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.513
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2624
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.883
_refine_diff_density_min         -0.69
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.03
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     750
_refine_ls_number_reflns         9829
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.03
_refine_ls_R_factor_all          0.1115
_refine_ls_R_factor_gt           0.0671
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0540P)^2^+1.7616P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1291
_refine_ls_wR_factor_ref         0.1482
_reflns_number_gt                6460
_reflns_number_total             9829
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic5009945_si_003.cif
_cod_data_source_block           1069sb13
_cod_depositor_comments
'Adding full bibliography for 4340733--4340738.cif.'
_cod_original_cell_volume        5578.2(3)
_cod_database_code               4340738