Bringing an important macrocycle into a polyoxometalate matrix: synthesis, crystal structure, spectroscopy and electrochemistry of [Co(III)(transdiene)(Cl)2]2[Mo6O19], [Ni(II)(transdiene)][W6O19]·DMSO·DCM and [Zn(II)(transdsiene)(Cl)]2[W6O19].
Sarma, Monima; Chatterjee, Tanmay; Das, Samar K.; Dalton transactions (Cambridge, England : 2003) 40 (2011) 2954–2966; doi:10.1039/c0dt01208d

data_7015117
_publ_section_title
;
 Bringing an important macrocycle into a polyoxometalate matrix:
 synthesis, crystal structure, spectroscopy and electrochemistry of
 [Co(III)(transdiene)(Cl)2]2[Mo6O19],
 [Ni(II)(transdiene)][W6O19]&#x00B7;DMSO&#x00B7;DCM and
 [Zn(II)(transdsiene)(Cl)]2[W6O19].
;
_journal_issue                   12
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2954
_journal_page_last               2966
_journal_paper_doi               10.1039/c0dt01208d
_journal_volume                  40
_journal_year                    2011
_chemical_formula_moiety
;
C16 H30 N4 Ni, O19 W6, C2 H6 O S, C H2 Cl2
;
_chemical_formula_sum            'C19 H38 Cl2 N4 Ni O20 S W6'
_chemical_formula_weight         1907.30
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 96.5540(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.1285(13)
_cell_length_b                   16.4933(12)
_cell_length_c                   12.8503(9)
_cell_measurement_reflns_used    5848
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.02
_cell_measurement_theta_min      2.22
_cell_volume                     3817.1(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  '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  0.0451
_diffrn_reflns_av_sigmaI/netI    0.0317
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            36003
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.67
_exptl_absorpt_coefficient_mu    18.761
_exptl_absorpt_correction_T_max  0.2118
_exptl_absorpt_correction_T_min  0.1533
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    3.319
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             3448
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.314
_refine_diff_density_min         -0.836
_refine_diff_density_rms         0.212
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.184
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     486
_refine_ls_number_reflns         6669
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.184
_refine_ls_R_factor_all          0.0380
_refine_ls_R_factor_gt           0.0337
_refine_ls_shift/su_max          0.027
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0165P)^2^+29.8497P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0607
_refine_ls_wR_factor_ref         0.0621
_reflns_number_gt                6206
_reflns_number_total             6669
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0dt01208d.txt
_cod_data_source_block           Ni-TDE-W6
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Empirical' changed to
'empirical' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1555 2011-01-17 13:19:09Z saulius 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7015117