A building block approach to the synthesis of organic‒inorganic oxide materials: the hydrothermal synthesis and network structure of [{Ni4(tpypyz)3}{Mo5O15(O3PCH2CH2PO3)}2]·23H2O (tpypyz = tetra-2-pyridylpyrazine)
Burkholder, Eric; Golub, Vladimir; O'Connor, Charles J.; Zubieta, Jon; Chemical Communications (Cambridge, United Kingdom)  (2003) 2128–2129; doi:10.1039/b303659f

data_7113850
_publ_section_title
;
 A building block approach to the synthesis of organic--inorganic oxide
 materials: the hydrothermal synthesis and network structure of
 [{Ni4(tpypyz)3}{Mo5O15(O3PCH2CH2PO3)}2]&#x00B7;23H2O
 (tpypyz = tetra-2-pyridylpyrazine)
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   17
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              2128
_journal_page_last               2129
_journal_paper_doi               10.1039/b303659f
_journal_year                    2003
_chemical_formula_sum            'C38 H51 Mo5 N9 Ni2 O32.5 P2'
_chemical_formula_weight         1812.94
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   24.6741(13)
_cell_length_b                   15.4148(8)
_cell_length_c                   30.8125(16)
_cell_measurement_reflns_used    21129
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      33.00
_cell_measurement_theta_min      1.32
_cell_volume                     11719.4(11)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL and CrystalMaker 5.x'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean '512 x 512'
_diffrn_measured_fraction_theta_full 0.956
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_device_type  'APEX CCD area 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  0.1421
_diffrn_reflns_av_sigmaI/netI    0.0997
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            152194
_diffrn_reflns_theta_full        33.00
_diffrn_reflns_theta_max         33.00
_diffrn_reflns_theta_min         1.32
_diffrn_standards_decay_%        <1%
_exptl_absorpt_coefficient_mu    1.820
_exptl_absorpt_correction_T_max  0.9645
_exptl_absorpt_correction_T_min  0.4631
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS SHELXL-97 (Sheldrick, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.055
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             7184
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.166
_refine_diff_density_min         -0.881
_refine_diff_density_rms         0.211
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     870
_refine_ls_number_reflns         21129
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.1249
_refine_ls_R_factor_gt           0.0720
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0463P)^2^+12.4564P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1179
_refine_ls_wR_factor_ref         0.1379
_reflns_number_gt                13734
_reflns_number_total             21129
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             7103855
_cod_data_source_file            b303659f.txt
_cod_data_source_block           pbca
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/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      Pbca
_cod_original_formula_sum        'C38 H51 Mo5 N9 Ni2 O32.50 P2'
_cod_database_code               7113850