A polyoxometallate-templated coordination polymer: synthesis and crystal structure of [Cu3(4,4′-bipy)5(MeCN)2]PW12O40·2C6H5CN
Inman, Chad; Knaust, Jacqueline M.; Keller, Steven W.; Chemical Communications  (2002) 156–; doi:10.1039/b107305b

data_7114083
_publ_section_title
;
 A polyoxometallate-templated coordination polymer: synthesis and crystal
 structure of [Cu3(4,4&#x2032;-bipy)5(MeCN)2]PW12O40&#x00B7;2C6H5CN
;
_journal_issue                   2
_journal_name_full               'Chemical Communications'
_journal_page_first              156
_journal_paper_doi               10.1039/b107305b
_journal_year                    2002
_chemical_formula_sum            'C68 H56 Cu3 N14 O40 P W12'
_chemical_formula_weight         4137.06
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 130.9800(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   51.552(2)
_cell_length_b                   14.1894(6)
_cell_length_c                   34.4299(15)
_cell_measurement_reflns_used    14064
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.0825
_cell_measurement_theta_min      2.2825
_cell_volume                     19013.3(14)
_computing_cell_refinement       'Smart (Bruker 1998)'
_computing_data_collection       'Smart (Bruker 1998)'
_computing_data_reduction        'Saint (Bruker 1998)'
_computing_molecular_graphics    'ORTEP-III (Burnett & Johnson, 1996)'
_computing_publication_material  'CIFTAB (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker SMART CCD area detector'
_diffrn_measurement_method       '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  0.0716
_diffrn_reflns_av_sigmaI/netI    0.0856
_diffrn_reflns_limit_h_max       66
_diffrn_reflns_limit_h_min       -59
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            67086
_diffrn_reflns_theta_full        27.11
_diffrn_reflns_theta_max         27.11
_diffrn_reflns_theta_min         1.53
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    15.210
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.472479
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Data were collected for decay and absorption using the program SADABS
based on the method of R.H. Blessing (Acta Cryst. A51, 33-38, 1995).
;
_exptl_crystal_colour            'deep yellow/orange'
_exptl_crystal_density_diffrn    2.854
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rectangular columns'
_exptl_crystal_F_000             14760
_exptl_crystal_size_max          .2
_exptl_crystal_size_mid          .13
_exptl_crystal_size_min          .1
_refine_diff_density_max         3.051
_refine_diff_density_min         -2.017
_refine_diff_density_rms         0.290
_refine_ls_extinction_coef       0.0000021(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1161
_refine_ls_number_reflns         20810
_refine_ls_number_restraints     130
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.1017
_refine_ls_R_factor_gt           0.0513
_refine_ls_shift/su_max          7.358
_refine_ls_shift/su_mean         0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0596P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1115
_refine_ls_wR_factor_ref         0.1275
_reflns_number_gt                13123
_reflns_number_total             20810
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b107305b.txt
_cod_data_source_block           u:\keller~1\chad\ci69b\work\ci69b
_cod_depositor_comments
;
The following automatic conversions were performed:
'__diffrn_measurement_device_type' tag replaced with
'_diffrn_measurement_device_type'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 

The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'multi-scans' was replaced
with the value 'multi-scan' as specified in the replacement file
'src/cod-tools/trunk/data/replacement-values/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 5376 2017-05-30 11:51:03Z andrius 
;
_cod_original_cell_volume        19013.4(14)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7114083