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_7119943
_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(C10 H19 Mn0.5 Mo3 O16), C3 H7 N O, 3(C16 H36 N)'
_chemical_formula_sum            'C71 H153 Mn Mo6 N4 O33'
_chemical_formula_weight         2221.55
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-05-20
_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                 92.869(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   27.6934(6)
_cell_length_b                   13.7969(3)
_cell_length_c                   24.7992(5)
_cell_measurement_reflns_used    13751
_cell_measurement_temperature    103.7
_cell_measurement_theta_max      29.3057
_cell_measurement_theta_min      3.16
_cell_volume                     9463.5(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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      103.7
_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  -39.00   14.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -15.9046  -77.0000 -150.0000 53

  2 omega   -4.00   22.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -15.9046   77.0000 -150.0000 26

  3 omega   -6.00   22.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -15.9046 -100.0000   60.0000 28

  4 omega  -69.00  -22.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -15.9046  -37.0000   30.0000 47

  5 omega  -41.00    2.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -15.9046  100.0000  119.0000 43

  6 omega  -49.00   33.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       21.1390  -77.0000  -30.0000 82

  7 omega   28.00   60.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       21.1390 -100.0000   60.0000 32

  8 omega  -48.00  -23.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       21.1390  -37.0000  -90.0000 25
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0096792000
_diffrn_orient_matrix_UB_12      0.0425770000
_diffrn_orient_matrix_UB_13      -0.0124264000
_diffrn_orient_matrix_UB_21      -0.0223443000
_diffrn_orient_matrix_UB_22      -0.0085115000
_diffrn_orient_matrix_UB_23      0.0119179000
_diffrn_orient_matrix_UB_31      0.0080116000
_diffrn_orient_matrix_UB_32      0.0275868000
_diffrn_orient_matrix_UB_33      0.0228649000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0469
_diffrn_reflns_av_unetI/netI     0.0571
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            53886
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.159
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.976
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89813
_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            orange
_exptl_crystal_density_diffrn    1.559
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       bar
_exptl_crystal_F_000             4592
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.743
_refine_diff_density_min         -1.453
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.148
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1055
_refine_ls_number_reflns         18547
_refine_ls_number_restraints     114
_refine_ls_restrained_S_all      1.152
_refine_ls_R_factor_all          0.0988
_refine_ls_R_factor_gt           0.0777
_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^)+(0.0484P)^2^+113.7000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1772
_refine_ls_wR_factor_ref         0.1900
_reflns_number_gt                14588
_reflns_number_total             18547
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7cc01971h2.cif
_cod_data_source_block           exp_3866
_cod_original_cell_volume        9463.5(4)
_cod_database_code               7119943
_reflns_odcompleteness_completeness 99.67
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32