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_7119944
_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
'C5 H11 Cr Mo6 O24.5, 5(C8 H18 N0.5), 0.5(C2 H8 N), 1.96055(C3 H7 N O), O'
_chemical_formula_sum            'C51.88 H118.72 Cr Mo6 N4.96 O27.46'
_chemical_formula_weight         1879.25
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-07-20
_audit_creation_method
;
  Olex2 1.1
  (compiled 2011.02.15 svn.r1672, GUI svn.r3494)
;
_audit_update_record
;
2017-02-20 deposited with the CCDC.
2017-04-11 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   24.6313(5)
_cell_length_b                   43.4932(13)
_cell_length_c                   14.5597(3)
_cell_measurement_reflns_used    12161
_cell_measurement_temperature    107.7
_cell_measurement_theta_max      70.9251
_cell_measurement_theta_min      3.0472
_cell_volume                     15597.7(6)
_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      107.7
_diffrn_detector_area_resol_mean 16.0971
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_details
;
  1 omega   24.00   59.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       -8.5000   15.0000  -30.0000 70

  2 omega  -18.00    9.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       -8.5000   45.0000  -60.0000 54

  3 omega   28.00  104.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7852   37.0000   30.0000 152

  4 omega   40.00   95.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7852   53.0000  132.0000 110

  5 omega  -31.00   -5.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7852  -37.0000 -150.0000 52

  6 omega   44.00   70.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7852 -103.0000 -100.0000 52

  7 omega   43.00   90.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000   30.0000 94

  8 omega   43.00   69.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000 -150.0000 52

  9 omega   92.00  161.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000  -60.0000 138

 10 omega   53.00   79.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000 -120.0000 52

 11 omega   65.00   95.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000   60.0000 60

 12 omega  141.00  169.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000   60.0000 56

 13 omega   40.00   98.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000  -30.0000 116

 14 omega   42.00   94.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000  150.0000 104
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0450600000
_diffrn_orient_matrix_UB_12      -0.0219995000
_diffrn_orient_matrix_UB_13      -0.0329232000
_diffrn_orient_matrix_UB_21      -0.0243779000
_diffrn_orient_matrix_UB_22      -0.0259464000
_diffrn_orient_matrix_UB_23      0.0593022000
_diffrn_orient_matrix_UB_31      -0.0358796000
_diffrn_orient_matrix_UB_32      -0.0099397000
_diffrn_orient_matrix_UB_33      -0.0811829000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0470
_diffrn_reflns_av_unetI/netI     0.0510
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -52
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            39033
_diffrn_reflns_theta_full        71.04
_diffrn_reflns_theta_max         71.04
_diffrn_reflns_theta_min         4.07
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.378
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.26258
_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    1.601
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             7683
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.18
_refine_diff_density_max         2.300
_refine_diff_density_min         -1.822
_refine_diff_density_rms         0.237
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     858
_refine_ls_number_reflns         14958
_refine_ls_number_restraints     446
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.1268
_refine_ls_R_factor_gt           0.1065
_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^)+(0.0854P)^2^+459.3000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2686
_refine_ls_wR_factor_ref         0.2835
_reflns_number_gt                11591
_reflns_number_total             14958
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7cc01971h2.cif
_cod_data_source_block           exp_4409
_cod_database_code               7119944
_reflns_odcompleteness_completeness 99.69
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97