Synthesis of novel bis(Triol)-functionalized Anderson clusters serving as potential synthons for forming organic-inorganic hybrid chains on purpose
Hao, Jian; Wei, Yongge; Xu, Qinghong; Yuan, Shanshan; Zhu, Li; Chem. Commun.  (2017) –; doi:10.1039/C7CC01971H

data_7119941
_publ_section_title
;
 Synthesis of novel bis(Triol)-functionalized Anderson clusters serving as
 potential synthons for forming organic-inorganic hybrid chains on purpose
;
_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C7CC01971H
_journal_year                    2017
_chemical_formula_moiety         'C10 H22 Cr2 K6 Mo12 O60, 3(O)'
_chemical_formula_sum            'C10 H22 Cr2 K6 Mo12 O63'
_chemical_formula_weight         2640.16
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-03-10
_audit_creation_method
;
  Olex2 1.1
  (compiled 2011.02.15 svn.r1672, GUI svn.r3494)
;
_audit_update_record
;
2017-03-10 deposited with the CCDC.
2017-04-11 downloaded from the CCDC.
;
_cell_angle_alpha                110.894(5)
_cell_angle_beta                 105.094(4)
_cell_angle_gamma                98.427(3)
_cell_formula_units_Z            2
_cell_length_a                   13.6143(5)
_cell_length_b                   15.9636(6)
_cell_length_c                   17.0731(12)
_cell_measurement_reflns_used    5092
_cell_measurement_temperature    104.9
_cell_measurement_theta_max      29.2017
_cell_measurement_theta_min      3.0013
_cell_volume                     3226.9(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_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
'A short history of SHELX (Sheldrick, 2007)/Bruker'
_diffrn_ambient_temperature      104.9
_diffrn_detector_area_resol_mean 16.0971
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega   -8.00   90.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       20.9827   77.0000  -60.0000 98

  2 omega   -8.00   30.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       20.9827   77.0000   60.0000 38

  3 omega  -50.00   42.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       20.9827  -37.0000   30.0000 92

  4 omega    5.00   70.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       20.9827 -137.0000 -177.0000 65

  5 omega   51.00   78.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       20.9827   37.0000   30.0000 27

  6 omega   -2.00   25.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       20.9827  -37.0000  -60.0000 27

  7 omega  -44.00   50.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       20.9827  -77.0000 -180.0000 94
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0011306000
_diffrn_orient_matrix_UB_12      0.0060009000
_diffrn_orient_matrix_UB_13      -0.0390091000
_diffrn_orient_matrix_UB_21      0.0366004000
_diffrn_orient_matrix_UB_22      0.0442443000
_diffrn_orient_matrix_UB_23      0.0266915000
_diffrn_orient_matrix_UB_31      0.0423759000
_diffrn_orient_matrix_UB_32      -0.0210668000
_diffrn_orient_matrix_UB_33      -0.0008799000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0555
_diffrn_reflns_av_unetI/netI     0.0975
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            25992
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.01
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.076
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77542
_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    2.717
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2504
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.01
_refine_diff_density_max         2.744
_refine_diff_density_min         -1.190
_refine_diff_density_rms         0.207
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     854
_refine_ls_number_reflns         12661
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.1101
_refine_ls_R_factor_gt           0.0650
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0522P)^2^+16.6100P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1336
_refine_ls_wR_factor_ref         0.1579
_reflns_number_gt                8117
_reflns_number_total             12661
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7cc01971h2.cif
_cod_data_source_block           exp_4646
_cod_database_code               7119941
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32