The proton-controlled synthesis of unprecedented diol functionalized Anderson-type POMs.
Zhang, Jiangwei; Li, Qi; Zeng, Mengyan; Huang, Yichao; Zhang, Jin; Hao, Jian; Wei, Yongge; Chemical communications (Cambridge, England) 52 (2016) 2378–2381; doi:10.1039/c5cc10071b

data_7118316
_publ_section_title
;
 The proton-controlled synthesis of unprecedented diol functionalized
 Anderson-type POMs.
;
_journal_issue                   11
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              2378
_journal_page_last               2381
_journal_paper_doi               10.1039/c5cc10071b
_journal_volume                  52
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_formula_moiety
'C3 H10 Cr Mo6 O25, Br, 4(C16 H36 N), 3(H2 O)'
_chemical_formula_sum            'C67 H161 Br Cr Mo6 N4 O28'
_chemical_formula_weight         2178.5455
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2015-08-12
_audit_creation_method
;
Olex2 1.2
(compiled 2014.06.27 svn.r2953 for OlexSys, GUI svn.r4855)
;
_audit_update_record
;
2015-09-07 deposited with the CCDC.
2015-12-16 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 93.071(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.5248(13)
_cell_length_b                   15.1876(6)
_cell_length_c                   18.3785(8)
_cell_measurement_reflns_used    15938
_cell_measurement_temperature    100
_cell_volume                     4605.9(5)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 16.0971
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0297
_diffrn_reflns_av_unetI/netI     0.0516
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            28622
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.18
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.402
_exptl_absorpt_correction_T_max  0.5407
_exptl_absorpt_correction_T_min  0.4866
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1923
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.5
_refine_diff_density_max         0.700
_refine_diff_density_min         -0.661
_refine_diff_density_rms         0.129
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.017(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     969
_refine_ls_number_reflns         17863
_refine_ls_number_restraints     62
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0575
_refine_ls_R_factor_gt           0.0465
_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^)+(0.0552P)^2^+18.7852P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0968
_refine_ls_wR_factor_ref         0.1046
_reflns_number_gt                13823
_reflns_number_total             17863
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5cc10071b2.cif
_cod_data_source_block           compound3
_cod_depositor_comments
'Adding full bibliography for 7118311--7118316.cif.'
_cod_original_cell_volume        4605.9(4)
_cod_database_code               7118316
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H2 of O2, H3 of O3, H15 of O15, H1AC of O1AA, All C(H,H)
  groups
 At 1.5 times of:
  All C(H,H,H) groups, H16 of O16, All O(H,H) groups
2. Restrained distances
 H9DB-H5AC
 2 with sigma of 0.02
 H9DB-H5AD
 2.1 with sigma of 0.01
 HB-H5AE
 2.1 with sigma of 0.01
 H3CA-H5AE
 2.1 with sigma of 0.01
 H9DB-H5AF
 2.1 with sigma of 0.01
 O15-H15
 0.8 with sigma of 0.01
 H7DA-H5AC
 2.1 with sigma of 0.01
 H0BA-HA
 2.1 with sigma of 0.01
 H6DA-H5AF
 2.1 with sigma of 0.01
 H9DB-H5AE
 2.1 with sigma of 0.01
 O16-C7
 1.41 with sigma of 0.01
3. Rigid bond restraints
 C2DA, C0EA
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C8CA, C9CA
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C6DA, C5EA
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C0BA, C3EA
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C9DA \\sim C2EA: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C9DA \\sim C2EA \\sim C6EA \\sim C7DA: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
C0EA \\sim C2DA \\sim C9AA \\sim C6BA: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
Uanis(O5AA) = Uanis(O5AB)
Uanis(C9DA) = Uanis(C2EA)
5. Others
 Sof(O5AB)=Sof(H5AE)=Sof(H5AF)=1-FVAR(1)
 Sof(O5AA)=Sof(H5AC)=Sof(H5AD)=FVAR(1)
6.a Free rotating group:
 O(HA,HB), O5AA(H5AC,H5AD), O5AB(H5AE,H5AF)
6.b Ternary CH refined with riding coordinates:
 O2(H2), O3(H3), O1AA(H1AC), C7(H7)
6.c Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C13(H13A,H13B), C4(H4A,H4B), C6(H6A,H6B), C10(H10A,H10B),
 C0AA(H0AA,H0AB), C9EA(H9EA,H9EB), C7EA(H7EA,H7EB), C16(H16A,H16B), C17(H17A,
 H17B), C1AA(H1AA,H1AB), C0FA(H0FA,H0FB), C4AA(H4AA,H4AB), C8(H8A,H8B), C9(H9A,
 H9B), C7AA(H7AA,H7AB), C2AA(H2AA,H2AB), C4BA(H4BA,H4BB), C1CA(H1CA,H1CB),
 C20(H20A,H20B), C1(H1A,H1B), C5BA(H5BA,H5BB), C0CA(H0CA,H0CB), C2CA(H2CA,H2CB),
  C9BA(H9BA,H9BB), C1BA(H1BA,H1BB), C5AA(H5AA,H5AB), C6BA(H6BA,H6BB), C2BA(H2BA,
 H2BB), C8AA(H8AA,H8AB), C9AA(H9AA,H9AB), C0BA(H0BA,H0BB), C14(H14A,H14B),
 C8BA(H8BA,H8BB), C3BA(H3BA,H3BB), C0DA(H0DA,H0DB), C1DA(H1DA,H1DB), C5CA(H5CA,
 H5CB), C2DA(H2DA,H2DB), C8DA(H8DA,H8DB), C8CA(H8CA,H8CB), C5DA(H5DA,H5DB),
 C3CA(H3CA,H3CB), C4CA(H4CA,H4CB), C6DA(H6DA,H6DB), C7DA(H7DA,H7DB), C5EA(H5EA,
 H5EB), C6EA(H6EA,H6EB), C3DA(H3DA,H3DB), C9DA(H9DA,H9DB)
6.d Idealised Me refined as rotating group:
 C6AA(H6AA,H6AB,H6AC), C5(H5A,H5B,H5C), C3AA(H3AA,H3AB,H3AC), C7BA(H7BA,H7BB,
 H7BC), C18(H18A,H18B,H18C), C6CA(H6CA,H6CB,H6CC), C7CA(H7CA,H7CB,H7CC),
 C9CA(H9CA,H9CB,H9CC), C4DA(H4DA,H4DB,H4DC), C19(H19A,H19B,H19C), C4EA(H4EA,
 H4EB,H4EC), C1EA(H1EA,H1EB,H1EC), C0EA(H0EA,H0EB,H0EC), C8EA(H8EA,H8EB,H8EC),
 C3EA(H3EA,H3EB,H3EC), C2EA(H2EA,H2EB,H2EC)
6.e Idealised tetrahedral OH refined as rotating group:
 O16(H16)
;