Complexation of metal carbonyl units with [α-PW11O39](7-) and [α2-P2W17O61](10-): insights into the chiral "twisted-sandwich" dimeric structures.
Zhao, Chongchao; Glass, Elliot N.; Sumliner, Jordan M.; Bacsa, John; Kim, Daniel Taehyun; Guo, Weiwei; Hill, Craig L.; Dalton transactions (Cambridge, England : 2003) 43 (2014) 4040–4047; doi:10.1039/c3dt53374c

data_7028494
_publ_section_title
;
 Complexation of metal carbonyl units with [\a-PW11O39](7-) and
 [\a2-P2W17O61](10-): insights into the chiral
 &quot;twisted-sandwich&quot; dimeric structures.
;
_journal_issue                   10
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4040
_journal_page_last               4047
_journal_paper_doi               10.1039/c3dt53374c
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C6 O86 P2 Re2 W23, 7(K), 4(Na), 23(O)'
_chemical_formula_sum            'C6 K7 Na4 O109 P2 Re2 W23'
_chemical_formula_weight         6844.61
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_date             2014-01-06
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736)
;
_audit_update_record
;
2014-01-09 # Formatted by publCIF
;
_cell_angle_alpha                76.506(2)
_cell_angle_beta                 84.428(2)
_cell_angle_gamma                82.631(2)
_cell_formula_units_Z            2
_cell_length_a                   13.0794(4)
_cell_length_b                   19.8716(6)
_cell_length_c                   21.3258(6)
_cell_measurement_reflns_used    9468
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      31.116
_cell_measurement_theta_min      2.212
_cell_volume                     5332.3(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0413
_diffrn_reflns_av_unetI/netI     0.0603
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            64578
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.514
_diffrn_reflns_theta_min         1.574
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    27.390
_exptl_absorpt_correction_T_max  0.3521
_exptl_absorpt_correction_T_min  0.0132
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption
 correction. wR2(int) was
 0.1148 before and 0.0834 after correction. The Ratio of minimum to maximum
 transmission is 0.0375. The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    4.263
_exptl_crystal_description       plate
_exptl_crystal_F_000             5934
_exptl_crystal_recrystallization_method
'The material was recrystallised from water.'
_exptl_crystal_size_max          0.355
_exptl_crystal_size_mid          0.268
_exptl_crystal_size_min          0.088
_refine_diff_density_max         4.748
_refine_diff_density_min         -5.419
_refine_diff_density_rms         0.563
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1443
_refine_ls_number_reflns         32520
_refine_ls_number_restraints     138
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0803
_refine_ls_R_factor_gt           0.0530
_refine_ls_shift/su_max          0.022
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0322P)^2^+319.6019P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1166
_refine_ls_wR_factor_ref         0.1358
_reflns_Friedel_coverage         0.000
_reflns_number_gt                24012
_reflns_number_total             32520
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3dt53374c.txt
_cod_data_source_block           zcc96
_cod_database_code               7028494
_shelxl_version_number           2013-3
_shelx_estimated_absorpt_t_max   0.197
_shelx_estimated_absorpt_t_min   0.037
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Na2 \\sim Na2': within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
Uanis(W26B) \\sim Ueq, Uanis(O26A) \\sim Ueq: with sigma of 0.002 and sigma for
terminal atoms of 0.002
Uanis(C6) \\sim Ueq: with sigma of 0.007 and sigma for terminal atoms of 0.007
Uanis(O15W) \\sim Ueq: with sigma of 0.007 and sigma for terminal atoms of 0.007
Uanis(O27W) \\sim Ueq: with sigma of 0.007 and sigma for terminal atoms of 0.007
Uanis(O1W) \\sim Ueq: with sigma of 0.007 and sigma for terminal atoms of 0.007
Uanis(O17W) \\sim Ueq: with sigma of 0.007 and sigma for terminal atoms of 0.007
Uanis(O9W) \\sim Ueq: with sigma of 0.007 and sigma for terminal atoms of 0.007
Uanis(O24W) \\sim Ueq: with sigma of 0.007 and sigma for terminal atoms of 0.007
Uanis(O12W) \\sim Ueq: with sigma of 0.007 and sigma for terminal atoms of 0.007
Uanis(O22W) \\sim Ueq: with sigma of 0.007 and sigma for terminal atoms of 0.007
Uanis(W22A) = Uanis(W22B)
Uanis(W23A) = Uanis(W23B)
Uanis(O26A) = Uanis(W26B)
Uanis(W25A) = Uanis(O25B)
Uanis(O51A) = Uanis(W51B)
Uanis(W21A) = Uanis(W21B)
Uanis(O21W) = Uanis(O21W)
Uanis(O21W) = Uanis(O21W)
Uanis(K6') = Uanis(K6)
Uanis(K2A) = Uanis(K2B)
2. Rigid body (RIGU) restrains
 W22A, W22B, O86, O69, W19
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O25B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 W18, W26B, W6
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 W18, W26B, O26A, W6
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 W10, W51B, O25B, W6, W18
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 Re2, C6, O78
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
3. Others
 Sof(K2B)=1-FVAR(1)
 Sof(K2A)=FVAR(1)
 Sof(W22B)=1-FVAR(2)
 Sof(W22A)=FVAR(2)
 Sof(W23B)=1-FVAR(3)
 Sof(W23A)=FVAR(3)
 Sof(W21B)=1-FVAR(4)
 Sof(W21A)=FVAR(4)
 Sof(K6)=1-FVAR(5)
 Sof(K6')=FVAR(5)
 Fixed Sof: W26B(0.05) W51B(0.05) O5W(0.5) O27W(0.5) O1W(0.5) O11W(0.5)
 O16W(0.5) O15W(0.5) W6(0.95) W10(0.95) W18(0.95) W25A(0.05) Na2'(0.5) Na2(0.5)
;