pH-dependent assembly of metal‒organic hybrid compounds based on octamolybdates and a new flexible multidentate ligand
Yue, Zhong-Cheng; Shen, Li-Xia; Wu, Huan-Huan; Li, Xing-Hui; Niu, Yun-Yin; CrystEngComm 15 (2013) 9938–; doi:10.1039/c3ce41223g

data_7211341
_publ_section_title
;
 pH-dependent assembly of metal--organic hybrid compounds based on
 octamolybdates and a new flexible multidentate ligand
;
_journal_issue                   46
_journal_name_full               CrystEngComm
_journal_page_first              9938
_journal_paper_doi               10.1039/c3ce41223g
_journal_volume                  15
_journal_year                    2013
_chemical_formula_moiety         'Cu H4 Mo16 O54, 2(C18 H20 N6), 2(H2 O)'
_chemical_formula_sum            'C36 H48 Cu Mo16 N12 O56'
_chemical_formula_weight         3143.44
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-03-22
_audit_creation_method
;
  Olex2 1.2
  (compiled Dec  5 2012 16:20:19, GUI svn.r4385)
;
_cell_angle_alpha                75.506(5)
_cell_angle_beta                 79.777(5)
_cell_angle_gamma                78.407(5)
_cell_formula_units_Z            1
_cell_length_a                   9.6510(6)
_cell_length_b                   10.4093(7)
_cell_length_c                   20.4141(12)
_cell_measurement_reflns_used    7355
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      26.3154
_cell_measurement_theta_min      2.9399
_cell_volume                     1927.5(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_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, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      291.15
_diffrn_detector_area_resol_mean 16.2312
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -11.00   20.00   1.0000    1.6000
omega____ theta____ kappa____ phi______ frames
    -      -17.1323 -108.0000   -7.0000 31

  2 omega  -13.00   24.00   1.0000    1.6000
omega____ theta____ kappa____ phi______ frames
    -      -17.1323  -99.0000   90.0000 37

  3 omega  -36.00   38.00   1.0000    1.6000
omega____ theta____ kappa____ phi______ frames
    -       19.7104  -57.0000 -180.0000 74

  4 omega   44.00   95.00   1.0000    1.6000
omega____ theta____ kappa____ phi______ frames
    -       19.7104 -178.0000    0.0000 51

  5 omega   -3.00   92.00   1.0000    1.6000
omega____ theta____ kappa____ phi______ frames
    -       19.7104   37.0000  120.0000 95

  6 omega  -47.00   46.00   1.0000    1.6000
omega____ theta____ kappa____ phi______ frames
    -       19.7104  -37.0000  -60.0000 93

  7 omega  -24.00   30.00   1.0000    1.6000
omega____ theta____ kappa____ phi______ frames
    -       19.7104   19.0000  -30.0000 54
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0035886000
_diffrn_orient_matrix_UB_12      0.0342346000
_diffrn_orient_matrix_UB_13      0.0263967000
_diffrn_orient_matrix_UB_21      0.0161545000
_diffrn_orient_matrix_UB_22      -0.0625126000
_diffrn_orient_matrix_UB_23      0.0231923000
_diffrn_orient_matrix_UB_31      0.0738786000
_diffrn_orient_matrix_UB_32      0.0033200000
_diffrn_orient_matrix_UB_33      -0.0087662000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0236
_diffrn_reflns_av_unetI/netI     0.0397
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            15880
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.95
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.889
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97461
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    2.708
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1497
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.109
_refine_diff_density_min         -0.821
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     551
_refine_ls_number_reflns         7842
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0448
_refine_ls_R_factor_gt           0.0323
_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^)+(0.0260P)^2^+1.1202P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0669
_refine_ls_wR_factor_ref         0.0730
_reflns_number_gt                6257
_reflns_number_total             7842
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce41223g.txt
_cod_data_source_block           nyy2013031804
_cod_database_code               7211341
_chemical_oxdiff_formula         C20H20N4O4Mo8Cu1
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  {H15A,H15B} of C15, H2 of C2, H10 of C10, {H11A,H11B} of C11, H16 of C16,
  H12 of C12, H18 of C18, H13 of C13, H4A of C4, H14 of C14, H9 of C9, H6 of C6,
   H4 of N4, {H7A,H7B} of C7, H17 of C17, H8 of C8, H6A of N6
 At 1.5 times of:
  {H28A,H28B} of O28, {H27A,H27B} of O27
2.a Free rotating group:
 O28(H28A,H28B)
2.b Rotating group:
 O27(H27A,H27B)
2.c Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C7(H7A,H7B), C15(H15A,H15B)
2.d Aromatic/amide H refined with riding coordinates:
 N4(H4), C2(H2), C4(H4A), C6(H6), C14(H14), N6(H6A), C12(H12), C18(H18),
 C16(H16), C13(H13), C17(H17), C8(H8), C9(H9), C10(H10)
;