Solid state coordination chemistry: Structural consequences of varying diphosphonate tether length and fluoride incorporation in the copper-bisterpy/oxomolybdenum/organodiphosphonate system (bisterpy = 2,2':4',4":2',2"'-quarterpyridyl-6',6'-di-2-pyridine)
Stephanie Jones; Jose M. Vargas; Steven Pellizzeri; Charles J. O-Connor; Jon Zubieta; Inorganica Chimica Acta 395 (2013) 44–57; doi:10.1016/j.ica.2012.10.023

data_1512855
_publ_section_title
;
 Solid state coordination chemistry: Structural consequences of varying
 diphosphonate tether length and fluoride incorporation in the
 copper-bisterpy/oxomolybdenum/organodiphosphonate system (bisterpy =
 2,2':4',4":2',2"'-quarterpyridyl-6',6'-di-2-pyridine)
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              44
_journal_page_last               57
_journal_paper_doi               10.1016/j.ica.2012.10.023
_journal_volume                  395
_journal_year                    2013
_chemical_formula_moiety         'C31 H45 Cu2 F3 Mo2 N6 O22 P2'
_chemical_formula_sum            'C31 H34 Cu2 F3 Mo2 N6 O16.5 P2'
_chemical_formula_weight         1192.55
_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
_cell_angle_alpha                86.836(2)
_cell_angle_beta                 78.190(2)
_cell_angle_gamma                84.923(2)
_cell_formula_units_Z            2
_cell_length_a                   9.4285(10)
_cell_length_b                   13.1589(13)
_cell_length_c                   15.9484(16)
_cell_measurement_reflns_used    2291
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      23.02
_cell_measurement_theta_min      2.33
_cell_volume                     1927.8(3)
_computing_cell_refinement       'Bruker SMART (Bruker, 2002)'
_computing_data_collection       'Bruker SMART (Bruker, 2002)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2002)'
_computing_molecular_graphics    'CrystalMaker (Palmer, 2006)'
_computing_publication_material  'Bruker SHELXTL (Bruker, 2002)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 512
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX CCD area detector'
_diffrn_measurement_method       'Phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0531
_diffrn_reflns_av_sigmaI/netI    0.0842
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            20116
_diffrn_reflns_theta_full        28.08
_diffrn_reflns_theta_max         28.08
_diffrn_reflns_theta_min         1.55
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        0.001
_exptl_absorpt_coefficient_mu    1.925
_exptl_absorpt_correction_T_max  0.8943
_exptl_absorpt_correction_T_min  0.5635
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS SHELXL-97 (Sheldrick, 1997)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.225
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.881
_refine_diff_density_min         -1.087
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.940
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     515
_refine_ls_number_reflns         9332
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.940
_refine_ls_R_factor_all          0.0725
_refine_ls_R_factor_gt           0.0479
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0484P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0991
_refine_ls_wR_factor_ref         0.1081
_reflns_number_gt                6668
_reflns_number_total             9332
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2013-395-44-57-3.cif
_cod_data_source_block           compound-3.11H2O
_cod_original_sg_symbol_Hall     -P1
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C31 H34 Cu2 F3 Mo2 N6 O16.50 P2'
_cod_database_code               1512855