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_7211340
_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         '3(Mo8 O26), 4(C18 H21 N6), 4(H2 O), 0.6(O)'
_chemical_formula_sum            'C72 H93.2 Mo24 N24 O82.6'
_chemical_formula_weight         4919.07
_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 Apr  9 2013 14:06:00, GUI svn.r4456)
;
_cell_angle_alpha                101.016(3)
_cell_angle_beta                 92.618(3)
_cell_angle_gamma                96.446(3)
_cell_formula_units_Z            1
_cell_length_a                   10.3022(3)
_cell_length_b                   12.5187(4)
_cell_length_c                   25.8195(11)
_cell_measurement_reflns_used    8846
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      29.2259
_cell_measurement_theta_min      2.9404
_cell_volume                     3240.2(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   25.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.1323  -99.0000 -150.0000 36

  2 omega  -76.00  -25.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.1323  128.0000 -101.0000 51

  3 omega  -80.00  -34.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.1323  141.0000   69.0000 46

  4 omega  -24.00   35.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7104  -57.0000   30.0000 59

  5 omega  -26.00   20.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7104  -57.0000 -150.0000 46

  6 omega  -52.00   93.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7104    0.0000   60.0000 145

  7 omega   -6.00   49.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7104   37.0000 -180.0000 55
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0255299000
_diffrn_orient_matrix_UB_12      0.0215075000
_diffrn_orient_matrix_UB_13      -0.0212906000
_diffrn_orient_matrix_UB_21      0.0269614000
_diffrn_orient_matrix_UB_22      -0.0400773000
_diffrn_orient_matrix_UB_23      -0.0182149000
_diffrn_orient_matrix_UB_31      -0.0586929000
_diffrn_orient_matrix_UB_32      -0.0362583000
_diffrn_orient_matrix_UB_33      -0.0013913000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0365
_diffrn_reflns_av_unetI/netI     0.0593
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            26832
_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    2.347
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95343
_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    2.521
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2362
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.663
_refine_diff_density_min         -0.824
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     923
_refine_ls_number_reflns         13242
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0645
_refine_ls_R_factor_gt           0.0378
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0194P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0623
_refine_ls_wR_factor_ref         0.0708
_reflns_number_gt                9602
_reflns_number_total             13242
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce41223g.txt
_cod_data_source_block           nyy134907a
_cod_original_formula_sum        'C72 H93.20 Mo24 N24 O82.60'
_cod_database_code               7211340
_chemical_oxdiff_formula         C20H20N4O4Mo1Fe1
_reflns_odcompleteness_completeness 99.85
_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(C17) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(O40) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O40) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C16) = Uanis(C17)
3. Others
 Fixed Sof: O42(0.3)
4.a Free rotating group:
 O40(H40A,H40B), O41(H41A,H41B)
4.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C25(H25A,H25B), C27(H27A,H27B), C7(H7A,H7B), C26(H26A,H26B),
 C9(H9A,H9B)
4.c Aromatic/amide H refined with riding coordinates:
 N4(H4), C15(H15), C30(H30), C20(H20), C14(H14), C35(H35), C24(H24), C31(H31),
 C13(H13), C22(H22), N2(H2), N12(H12A), C2(H2A), C11(H11), C29(H29), C10(H10),
 N10(H10A), C32(H32), C36(H36), C12(H12), C4(H4A), C28(H28), C33(H33), C6(H6),
 C34(H34), N6(H6A), C18(H18), C16(H16), C17(H17)
;