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_7211344
_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         'Co H4 Mo16 O54, 2(O), 2(C18 H21 N6)'
_chemical_formula_sum            'C36 H50 Co Mo16 N12 O56'
_chemical_formula_weight         3140.85
_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             2013-04-12
_audit_creation_method
;
  Olex2 1.2
  (compiled Mar 21 2013 11:16:32, GUI svn.r4446)
;
_cell_angle_alpha                104.412(4)
_cell_angle_beta                 95.009(3)
_cell_angle_gamma                101.078(3)
_cell_formula_units_Z            1
_cell_length_a                   9.6394(4)
_cell_length_b                   10.3809(4)
_cell_length_c                   20.3352(8)
_cell_measurement_reflns_used    7800
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      26.3149
_cell_measurement_theta_min      3.1285
_cell_volume                     1914.45(14)
_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   -9.00   29.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -17.1323 -113.0000    2.0000 38

  2 omega    0.00   37.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       19.7104   57.0000  -60.0000 37

  3 omega   39.00   79.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       19.7104  178.0000   90.0000 40

  4 omega  -50.00   45.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       19.7104  -77.0000   90.0000 95

  5 omega  -40.00   39.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       19.7104  -57.0000  -60.0000 79

  6 omega    3.00   89.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       19.7104   57.0000 -150.0000 86

  7 omega   35.00   94.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       19.7104  178.0000  -60.0000 59
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0246616000
_diffrn_orient_matrix_UB_12      0.0651695000
_diffrn_orient_matrix_UB_13      0.0237627000
_diffrn_orient_matrix_UB_21      0.0232496000
_diffrn_orient_matrix_UB_22      0.0274818000
_diffrn_orient_matrix_UB_23      -0.0268130000
_diffrn_orient_matrix_UB_31      -0.0677446000
_diffrn_orient_matrix_UB_32      0.0152241000
_diffrn_orient_matrix_UB_33      -0.0063354000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0223
_diffrn_reflns_av_unetI/netI     0.0352
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            15733
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.13
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.847
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94119
_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    2.724
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1497
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.839
_refine_diff_density_min         -0.846
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     552
_refine_ls_number_reflns         7794
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0384
_refine_ls_R_factor_gt           0.0291
_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^)+(0.0246P)^2^+1.5604P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0633
_refine_ls_wR_factor_ref         0.0676
_reflns_number_gt                6480
_reflns_number_total             7794
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce41223g.txt
_cod_data_source_block           nyy134901
_cod_original_cell_volume        1914.46(13)
_cod_database_code               7211344
_chemical_oxdiff_formula         C20H20N4O4Mo4Co1
_reflns_odcompleteness_completeness 99.77
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O28) = Uanis(O28A)
3. Others
 Sof(O28)=1-Sof(O28A)
4.a Rotating group:
 O1(H1A,H1B)
4.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B)
4.c Aromatic/amide H refined with riding coordinates:
 N2(H2), N4(H4), N6(H6), C2(H2A), C4(H4A), C6(H6A), C10(H10), C11(H11),
 C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18)
;