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_7119942
_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
'2(C5 H11 Cr0.5 Mo3 O14), 3(C16 H36 N), 4(H O0.5)'
_chemical_formula_sum            'C58 H134 Cr Mo6 N3 O30'
_chemical_formula_weight         1981.32
_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             2017-02-28
_audit_creation_method
;
  Olex2 1.1
  (compiled 2011.02.15 svn.r1672, GUI svn.r3494)
;
_audit_update_record
;
2017-03-01 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            4
_cell_length_a                   27.1536(16)
_cell_length_b                   24.9590(9)
_cell_length_c                   13.8885(8)
_cell_measurement_reflns_used    5172
_cell_measurement_temperature    105.9
_cell_measurement_theta_max      29.1572
_cell_measurement_theta_min      3.1036
_cell_volume                     9412.6(8)
_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      105.9
_diffrn_detector_area_resol_mean 16.0971
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega  -72.00   -4.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.0609  -55.0000   -7.0000 68

  2 omega  -16.00   52.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.0609   77.0000  -90.0000 68

  3 omega   16.00   72.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       21.1390 -132.0000  172.0000 56
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0148355000
_diffrn_orient_matrix_UB_12      0.0099071000
_diffrn_orient_matrix_UB_13      0.0232767000
_diffrn_orient_matrix_UB_21      0.0303757000
_diffrn_orient_matrix_UB_22      -0.0188541000
_diffrn_orient_matrix_UB_23      0.0118564000
_diffrn_orient_matrix_UB_31      0.0382539000
_diffrn_orient_matrix_UB_32      0.0188269000
_diffrn_orient_matrix_UB_33      -0.0003619000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0667
_diffrn_reflns_av_unetI/netI     0.0843
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            27952
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.11
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.950
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76695
_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    1.398
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4076
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.13
_platon_squeeze_details
;
;
_refine_diff_density_max         1.852
_refine_diff_density_min         -1.623
_refine_diff_density_rms         0.176
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     588
_refine_ls_number_reflns         8473
_refine_ls_number_restraints     348
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.1644
_refine_ls_R_factor_gt           0.1229
_refine_ls_shift/su_max          0.043
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1200P)^2^+160.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2985
_refine_ls_wR_factor_ref         0.3233
_reflns_number_gt                5152
_reflns_number_total             8473
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7cc01971h2.cif
_cod_data_source_block           exp_4607
_cod_database_code               7119942
_reflns_odcompleteness_completeness 99.58
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32