β-{Cr[RC(CH2O)3]2Mo6O18}3−: the first organically-functionalized β isomer of Anderson-type polyoxometalates
Zhang, Jiangwei; Huang, Yichao; Hao, Jian; Wei, Yongge; Inorganic Chemistry Frontiers 4 (2017) 1215–; doi:10.1039/C7QI00199A

data_4349708
_publ_section_title
;
 \b-{Cr[RC(CH2O)3]2Mo6O18}3&#x2212;: the first organically-functionalized
 \b isomer of Anderson-type polyoxometalates
;
_journal_issue                   7
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              1215
_journal_paper_doi               10.1039/C7QI00199A
_journal_volume                  4
_journal_year                    2017
_chemical_formula_moiety
'C12 H22 Cr Mo6 O24, 2(C16 H36 N), H4 N, 2(H2 O)'
_chemical_formula_sum            'C44 H102 Cr Mo6 N3 O26'
_chemical_formula_weight         1716.93
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-10-01
_audit_creation_method
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_audit_update_record
;
2016-01-17 deposited with the CCDC.
2017-05-23 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 100.651(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.8005(4)
_cell_length_b                   35.9582(13)
_cell_length_c                   14.4617(4)
_cell_measurement_reflns_used    5180
_cell_measurement_temperature    103(0)
_cell_measurement_theta_max      29.2378
_cell_measurement_theta_min      3.0141
_cell_volume                     6541.8(4)
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      103(0)
_diffrn_detector_area_resol_mean 16.0971
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_details
;
  1 omega  -40.00   -8.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -15.9831   77.0000 -180.0000 32

  2 omega    9.00   36.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -15.9831 -118.0000   94.0000 27

  3 omega  -37.00   14.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       21.2956  -37.0000  -60.0000 51

  4 omega  -48.00   38.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       21.2956  -37.0000 -120.0000 86
;
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_orient_matrix_UB_11      0.0024424000
_diffrn_orient_matrix_UB_12      -0.0144362000
_diffrn_orient_matrix_UB_13      -0.0329562000
_diffrn_orient_matrix_UB_21      0.0089217000
_diffrn_orient_matrix_UB_22      -0.0131582000
_diffrn_orient_matrix_UB_23      0.0371777000
_diffrn_orient_matrix_UB_31      -0.0556225000
_diffrn_orient_matrix_UB_32      -0.0027060000
_diffrn_orient_matrix_UB_33      -0.0048568000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_av_unetI/netI     0.0317
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            6026
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.07
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.351
_exptl_absorpt_correction_T_max  0.667
_exptl_absorpt_correction_T_min  0.528
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.744
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3436.6
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.572
_refine_diff_density_min         -0.440
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     750
_refine_ls_number_reflns         12752
_refine_ls_number_restraints     182
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0606
_refine_ls_R_factor_gt           0.0585
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+332.4930P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1084
_refine_ls_wR_factor_ref         0.1095
_reflns_number_gt                11270
_reflns_number_total             12752
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7qi00199a2.cif
_cod_data_source_block           compound3
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4349708
_reflns_odcompleteness_completeness 80.69
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 C30-C31
 1.53 with sigma of 0.02
 C19-C20
 1.53 with sigma of 0.02
 H20B-H18A
 1.6 with sigma of 0.02
 H18A-H20B
 1.8 with sigma of 0.02
 C8-C10 = C9-C10 = C11-C10 = C12-C11 = C4-C3 = C4-C1 = C5-C4 = C6-C5
 1.53 with sigma of 0.02
 C24-C23 = C22-C21 = C28-C27 = C26-C25 = C19-C18 = C18-C17 = C14-C13 = C15-C14
 = C16-C15
 1.53 with sigma of 0.02
 C44-C43 = C43-C42 = C42-C41 = C40-C39 = C38-C37 = C36-C35 = C34-C33 = C32-C31
 = C30-C29
 1.53 with sigma of 0.02
 C30-C32
 2.5 with sigma of 0.01
 C31-C29
 2.5 with sigma of 0.01
 N3-H3D = N3-H3F = N3-H3E = N3-H3C
 0.8 with sigma of 0.01
 C41-C33
 2.5 with sigma of 0.02
 C41-C29
 2.5 with sigma of 0.01
 H3C-H3D \\sim H3C-H3E \\sim H3C-H3F \\sim H3D-H3E \\sim H3D-H3F \\sim H3E-H3F
 with sigma of 0.02
3. Rigid bond restraints
 C17, C22, C18, C6, C23, C14, C24, C44, C29, N3, C27, C26, C30, C15, C16, C28,
 C19, C31, C12, C32, C20
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N1, C13
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N1, C17
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C21, C22
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N2, C29
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O1, Mo3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C4, C5, C6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(Cr1) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O20) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(O7) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(O9) \\sim
Ueq, Uanis(O3) \\sim Ueq, Uanis(O10) \\sim Ueq, Uanis(O11) \\sim Ueq, Uanis(O5)
\\sim Ueq, Uanis(O14) \\sim Ueq, Uanis(O16) \\sim Ueq, Uanis(O22) \\sim Ueq,
Uanis(O24) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C8) \\sim
Ueq, Uanis(C9) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C11) \\sim Ueq,
Uanis(C42) \\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(O18) \\sim Ueq, Uanis(O19)
\\sim Ueq, Uanis(O21) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(N1) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C17)
\\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C22) \\sim Ueq,
Uanis(C23) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C26)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C35) \\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C38)
\\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C5) \\sim Ueq,
Uanis(C16) \\sim Ueq, Uanis(C28) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O8) \\sim Ueq, Uanis(O13) \\sim Ueq, Uanis(O15) \\sim Ueq, Uanis(C6)
\\sim Ueq, Uanis(O23) \\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(C31) \\sim Ueq:
with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C18) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(C43) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
Uanis(O17) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C29)
\\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(C27) \\sim Ueq: with sigma of 0.0001 and
sigma for terminal atoms of 0.0002
Uanis(O12) \\sim Ueq: with sigma of 0 and sigma for terminal atoms of 0
Uanis(O9) = Uanis(O12)
Uanis(C31) = Uanis(C32)
Uanis(C27) = Uanis(C28)
Uanis(C43) = Uanis(C44)
Uanis(N2) = Uanis(C41)
Uanis(C38) = Uanis(C39)
Uanis(C13) = Uanis(C14)
Uanis(O25) = Uanis(O1)
Uanis(O10) = Uanis(O8)
5. Others
 Fixed Uiso: H3C(0.1) H3D(0.1) H3E(0.1) H3F(0.1)
6.a Free rotating group:
 O25(H25C,H25D)
6.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C9(H9A,H9B), C3(H3A,H3B), C7(H7A,H7B), C8(H8A,H8B), C37(H37A,
 H37B), C11(H11A,H11B), C38(H38A,H38B), C2(H2A,H2B), C5(H5A,H5B), C41(H41A,
 H41B), C42(H42A,H42B), C43(H43A,H43B), C33(H33A,H33B), C34(H34A,H34B),
 C39(H39A,H39B), C35(H35A,H35B), C21(H21A,H21B), C25(H25A,H25B), C13(H13A,H13B),
  C17(H17A,H17B), C22(H22A,H22B), C18(H18A,H18B), C23(H23A,H23B), C14(H14A,
 H14B), C29(H29A,H29B), C27(H27A,H27B), C26(H26A,H26B), C30(H30A,H30B),
 C15(H15A,H15B), C19(H19A,H19B), C31(H31A,H31B)
6.c Idealised Me refined as rotating group:
 C36(H36A,H36B,H36C), C40(H40A,H40B,H40C), C6(H6A,H6B,H6C), C24(H24A,H24B,
 H24C), C44(H44A,H44B,H44C), C16(H16A,H16B,H16C), C28(H28A,H28B,H28C), C12(H12A,
 H12B,H12C), C32(H32A,H32B,H32C), C20(H20A,H20B,H20C)
;