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_1512853
_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         'C34 H29 Cu2 Mo5 N6 O22 P2, 4(H2O), O0.50'
_chemical_formula_sum            'C34 H39 Cu2 Mo5 N6 O26.5 P2'
_chemical_formula_weight         1624.43
_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                100.314(3)
_cell_angle_beta                 104.841(3)
_cell_angle_gamma                90.885(3)
_cell_formula_units_Z            2
_cell_length_a                   10.4478(16)
_cell_length_b                   15.021(2)
_cell_length_c                   15.994(2)
_cell_measurement_reflns_used    9450
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      31.81
_cell_measurement_theta_min      2.52
_cell_volume                     2382.1(6)
_computing_cell_refinement       'Bruker APEX2 (Bruker, 2011)'
_computing_data_collection       'Bruker APEX2 (Bruker, 2011)'
_computing_data_reduction        'Bruker APEX2 (Bruker, 2011)'
_computing_molecular_graphics    'CrystalMaker (Palmer,  2010)'
_computing_publication_material  'Bruker SHELXTL (Bruker, 2011)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker APEX II CCD detector'
_diffrn_measurement_method       'phi and omega 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  0.0182
_diffrn_reflns_av_sigmaI/netI    0.0162
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            51777
_diffrn_reflns_theta_full        28.08
_diffrn_reflns_theta_max         28.08
_diffrn_reflns_theta_min         1.38
_exptl_absorpt_coefficient_mu    2.315
_exptl_absorpt_correction_T_max  0.9248
_exptl_absorpt_correction_T_min  0.7202
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Bruker APEX2 (Bruker, 2011)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.265
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1590
_exptl_crystal_size_max          0.354
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.071
_refine_diff_density_max         0.787
_refine_diff_density_min         -0.765
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.763
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     729
_refine_ls_number_reflns         11422
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      0.763
_refine_ls_R_factor_all          0.0225
_refine_ls_R_factor_gt           0.0196
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0806
_refine_ls_wR_factor_ref         0.0856
_reflns_number_gt                10469
_reflns_number_total             11422
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2013-395-44-57-1.cif
_cod_data_source_block           compound-1.4.5H2O
_cod_original_sg_symbol_Hall     -P1
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C34 H39 Cu2 Mo5 N6 O26.50 P2'
_cod_database_code               1512853