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_4349709
_publ_section_title
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 \b-{Cr[RC(CH2O)3]2Mo6O18}3&#x2212;: the first organically-functionalized
 \b isomer of Anderson-type polyoxometalates
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_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         'C8 H18 Cr Mo6 N2 O24, H4 N'
_chemical_formula_sum            'C8 H22 Cr Mo6 N3 O24'
_chemical_formula_weight         1171.93
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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                 109.860(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   26.997(3)
_cell_length_b                   17.922(2)
_cell_length_c                   16.364(2)
_cell_measurement_reflns_used    3313
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.36
_cell_measurement_theta_min      3.32
_cell_volume                     7446.7(16)
_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  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.0971
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0953
_diffrn_reflns_av_unetI/netI     0.1182
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            18717
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.12
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.314
_exptl_absorpt_correction_T_max  0.5436
_exptl_absorpt_correction_T_min  0.3908
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    2.091
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4464
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.037
_refine_diff_density_min         -1.031
_refine_diff_density_rms         0.356
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     384
_refine_ls_number_reflns         7297
_refine_ls_number_restraints     138
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0547
_refine_ls_R_factor_gt           0.0434
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0851P)^2^+507.8282P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0882
_refine_ls_wR_factor_ref         0.0987
_reflns_number_gt                5135
_reflns_number_total             7297
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7qi00199a2.cif
_cod_data_source_block           compound1
_cod_original_cell_volume        7446.8(15)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4349709
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H,H) groups
2. Restrained distances
 N3-H3F = N3-H3D
 0.8 with sigma of 0.01
 N2-C4 = N1-C8
 1.47 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. Uiso/Uaniso restraints and constraints
Mo2 \\sim Mo3 \\sim Mo1: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
Uanis(C6) \\sim Ueq, Uanis(C4) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C6) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(O19) \\sim Ueq, Uanis(C4) \\sim
Ueq, Uanis(C8) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(O12)
\\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C1) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(O19) \\sim
Ueq, Uanis(O12) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of
0.1
Uanis(C1) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(O7) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(C1) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(O1) \\sim Ueq, Uanis(O7) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C4) \\sim
Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4. Others
 Fixed Uiso: H3C(0.01) H3D(0.01) H3E(0.01) H3F(0.01)
5.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C1(H1A,H1B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C3(H3A,H3B)
5.b Idealised Me refined as rotating group:
 N2(H2C,H2D,H2E), N1(H1C,H1D,H1E)
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