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_7028495
_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, 3(C3 H10 N), 2(C3 H9 N), 2(Na), 1.5(O), 1.5(H2 O)'
_chemical_formula_sum            'C21 H56 N5 Na2 O89 P2 Re2 W23'
_chemical_formula_weight         6511.58
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2014-01-05
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.0635(18)
_cell_length_b                   26.1690(19)
_cell_length_c                   38.199(3)
_cell_measurement_reflns_used    9256
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.68
_cell_measurement_theta_min      2.205
_cell_volume                     23055(3)
_computing_cell_refinement       'SAINT v8.32B (Bruker, 2013)'
_computing_data_collection       'APEX2 v2013.6-2 (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.32B (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 512
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.999
_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  0.1409
_diffrn_reflns_av_unetI/netI     0.1251
_diffrn_reflns_Laue_measured_fraction_full 0.965
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            90059
_diffrn_reflns_point_group_measured_fraction_full 0.965
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.682
_diffrn_reflns_theta_min         1.292
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    25.064
_exptl_absorpt_correction_T_max  0.3685
_exptl_absorpt_correction_T_min  0.0449
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1034 before and 0.0795 after correction.
The Ratio of minimum to maximum transmission is 0.1218.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    3.752
_exptl_crystal_description       needle
_exptl_crystal_F_000             22664
_exptl_crystal_recrystallization_method
'The material was crystallised from water.'
_exptl_crystal_size_max          0.534
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.064
_refine_diff_density_max         5.050
_refine_diff_density_min         -3.344
_refine_diff_density_rms         0.677
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1336
_refine_ls_number_reflns         21865
_refine_ls_number_restraints     1968
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.1951
_refine_ls_R_factor_gt           0.1000
_refine_ls_shift/su_max          0.055
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0725P)^2^+5102.6606P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2082
_refine_ls_wR_factor_ref         0.2679
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10539
_reflns_number_total             21865
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3dt53374c.txt
_cod_data_source_block           pw11reco
_cod_database_code               7028495
_shelxl_version_number           2013-3
_shelx_estimated_absorpt_t_max   0.297
_shelx_estimated_absorpt_t_min   0.026
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 N2S-C5S = N2S-C6S = N2S-C4S
 1.475 with sigma of 0.02
 N3S-C7S = N3S-C9S = N3S-C8S
 1.475 with sigma of 0.02
 N1S-C1S = N1S-C2S = N1S-C3S
 1.475 with sigma of 0.02
 N5S-C14S = N5S-C13S = N5S-C15S
 1.475 with sigma of 0.02
 C9S-C8S \\sim C9S-C7S \\sim C8S-C7S
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C4) \\sim Ueq, Uanis(C5) \\sim Ueq: with sigma of 0.007 and sigma for
terminal atoms of 0.007
Uanis(O4W) \\sim Ueq, Uanis(O5W) \\sim Ueq: with sigma of 0.007 and sigma for
terminal atoms of 0.007
Uanis(O2W) \\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
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Others
 Fixed Sof: O1W(0.5) O2W(0.5) O4W(0.5) O5W(0.5) H5WA(0.5) H5WB(0.5)
6.a Free rotating group:
 O3W(H3WA,H3WB), O5W(H5WA,H5WB)
6.b Ternary CH refined with riding coordinates:
 N1S(H1S), N2S(H2S), N5S(H5S)
6.c Idealised Me refined as rotating group:
 C1S(H1SA,H1SB,H1SC), C2S(H2SA,H2SB,H2SC), C3S(H3SA,H3SB,H3SC), C4S(H4SA,H4SB,
 H4SC), C5S(H5SA,H5SB,H5SC), C6S(H6SA,H6SB,H6SC), C7S(H7SA,H7SB,H7SC), C8S(H8SA,
 H8SB,H8SC), C9S(H9SA,H9SB,H9SC), C10S(H10A,H10B,H10C), C11S(H11A,H11B,H11C),
 C12S(H12A,H12B,H12C), C13S(H13A,H13B,H13C), C14S(H14A,H14B,H14C), C15S(H15A,
 H15B,H15C)
;