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_7028496
_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 Mn2 O86 P2 W23, 6(C3 H10 N), K3, 12.5(H2O)'
_chemical_formula_sum            'C24 H85 K3 Mn2 N6 O98.5 P2 W23'
_chemical_formula_weight         6551.65
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_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
_audit_creation_date             2014-01-03
_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                 127.936(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   57.054(8)
_cell_length_b                   13.2708(18)
_cell_length_c                   36.998(5)
_cell_measurement_reflns_used    9887
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.704
_cell_measurement_theta_min      2.159
_cell_volume                     22094(5)
_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_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      173.15
_diffrn_detector_area_resol_mean 512
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0570
_diffrn_reflns_av_unetI/netI     0.0486
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       74
_diffrn_reflns_limit_h_min       -74
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            108179
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.877
_diffrn_reflns_theta_min         1.396
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    24.313
_exptl_absorpt_correction_T_max  0.3005
_exptl_absorpt_correction_T_min  0.0388
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
The crystal faces were indexed and the distances of the faces were carefully
measured for a numerical absorption correction.
A combination of a numerical and multi-scan correction with inter-frame
scaling was performed using the program
SADABS-2012/1 (Bruker,2012).
wR2(int) was 0.0785 before and 0.0591 after correction.
The Ratio of minimum to maximum transmission is 0.1291.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    3.939
_exptl_crystal_description       prism
_exptl_crystal_F_000             23184
_exptl_crystal_recrystallization_method
'The material was recrystallised from water.'
_exptl_crystal_size_max          0.334
_exptl_crystal_size_mid          0.146
_exptl_crystal_size_min          0.091
_refine_diff_density_max         3.646
_refine_diff_density_min         -2.483
_refine_diff_density_rms         0.337
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1453
_refine_ls_number_reflns         26360
_refine_ls_number_restraints     144
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0502
_refine_ls_R_factor_gt           0.0366
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0341P)^2^+424.0826P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0798
_refine_ls_wR_factor_ref         0.0868
_reflns_Friedel_coverage         0.000
_reflns_number_gt                21142
_reflns_number_total             26360
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3dt53374c.txt
_cod_data_source_block           pw11mnco
_cod_original_formula_sum        'C24 H85 K3 Mn2 N6 O98.50 P2 W23'
_cod_database_code               7028496
_shelxl_version_number           2013-3
_shelx_estimated_absorpt_t_max   0.348
_shelx_estimated_absorpt_t_min   0.045
_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
2. Uiso/Uaniso restraints and constraints
Uanis(K1) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.002
Uanis(O11W) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(O14W) = Uanis(O15W)
Uanis(K3A) = Uanis(K3B)
Uiso(O5WA) = Uiso(O5WB)
3. Rigid body (RIGU) restrains
 N4, C10C, C11C, C12C
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C3C, C1C, N1, C2C
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 N6, C13C, C14C, C15C
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 N5, C16C, C17C, C18C
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C8C, C7C, N3, C9C
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 Mn1, C2, O79
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C6, O86
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C1, O78
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 Mn2, C4, O84
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 Mn2, C3, O83
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 Mn2, C5, O85
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
4. Others
 Sof(O15W)=1-FVAR(1)
 Sof(O14W)=FVAR(1)
 Sof(K3B)=1-FVAR(2)
 Sof(K3A)=FVAR(2)
 Sof(O5WB)=1-FVAR(3)
 Sof(O5WA)=FVAR(3)
5.a Ternary CH refined with riding coordinates:
 N1(H1), N2(H2), N3(H3), N4(H4), N6(H6), N5(H5)
5.b Idealised Me refined as rotating group:
 C1C(H1CA,H1CB,H1CC), C2C(H2CA,H2CB,H2CC), C3C(H3CA,H3CB,H3CC), C4C(H4CA,H4CB,
 H4CC), C5C(H5CA,H5CB,H5CC), C6C(H6CA,H6CB,H6CC), C7C(H7CA,H7CB,H7CC), C8C(H8CA,
 H8CB,H8CC), C9C(H9CA,H9CB,H9CC), C10C(H10A,H10B,H10C), C11C(H11A,H11B,H11C),
 C12C(H12A,H12B,H12C), C13C(H13A,H13B,H13C), C14C(H14A,H14B,H14C), C15C(H15A,
 H15B,H15C), C16C(H16A,H16B,H16C), C17C(H17A,H17B,H17C), C18C(H18A,H18B,H18C)
;