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_7211343
_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         '0.5(C72 H72 Cu4 Mo16 N24 O56), O'
_chemical_formula_sum            'C36 H42 Cu2 Mo8 N12 O29'
_chemical_formula_weight         2001.42
_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             2013-03-25
_audit_creation_method
;
  Olex2 1.2
  (compiled Dec  5 2012 16:20:19, GUI svn.r4385)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 115.844(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.4044(6)
_cell_length_b                   22.5801(8)
_cell_length_c                   11.8951(6)
_cell_measurement_reflns_used    5444
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      26.3104
_cell_measurement_theta_min      3.2879
_cell_volume                     2756.8(3)
_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  -12.00   25.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.1323  -99.0000  -30.0000 37

  2 omega  -62.00  -25.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.1323  124.0000  105.0000 37

  3 omega  -42.00   39.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7104  -57.0000   90.0000 81

  4 omega  -11.00   57.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7104    0.0000   90.0000 68

  5 omega   -6.00   19.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7104   37.0000  150.0000 25
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0626573000
_diffrn_orient_matrix_UB_12      0.0126499000
_diffrn_orient_matrix_UB_13      0.0185481000
_diffrn_orient_matrix_UB_21      0.0267327000
_diffrn_orient_matrix_UB_22      -0.0286481000
_diffrn_orient_matrix_UB_23      0.0032234000
_diffrn_orient_matrix_UB_31      -0.0118212000
_diffrn_orient_matrix_UB_32      0.0022309000
_diffrn_orient_matrix_UB_33      -0.0635453000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0336
_diffrn_reflns_av_unetI/netI     0.0519
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            12576
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.31
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.610
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94812
_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    2.411
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1936
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.647
_refine_diff_density_min         -0.888
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     401
_refine_ls_number_reflns         5626
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.0494
_refine_ls_R_factor_gt           0.0355
_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^)+(0.0196P)^2^+2.6434P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0669
_refine_ls_wR_factor_ref         0.0715
_reflns_number_gt                4614
_reflns_number_total             5626
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce41223g.txt
_cod_data_source_block           nyy2013031802
_cod_original_cell_volume        2756.8(2)
_cod_database_code               7211343
_chemical_oxdiff_formula         C20H20N4O4Mo8Cu1
_reflns_odcompleteness_completeness 99.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  H1 of C1, H18 of C18, H17 of C17, {H7A,H7B} of C7, {H2A,H2B} of C2, H15 of
  C15, H8 of C8, {H11A,H11B} of C11, H9 of C9, H16 of C16, H4 of C4, H14 of C14,
   H12 of C12, H6 of C6, H13 of C13
2. Restrained distances
 Cu1-O14A
 2.1 with sigma of 0.02
 Cu1-O14
 2.2 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O14) ~ Ueq: with sigma of 0.008 and sigma for terminal atoms of 0.008
Uanis(O14) = Uanis(O14A)
4. Others
 Sof(O14)=1-Sof(O14A)
 Fixed Sof: O15(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C7(H7A,H7B), C11(H11A,H11B)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C4(H4), C6(H6), C8(H8), C9(H9), C12(H12), C13(H13), C14(H14),
 C15(H15), C16(H16), C17(H17), C18(H18)
;