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_7211342
_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         'Mo8 O26, C36 H38 Cu N12, 4(H2 O)'
_chemical_formula_sum            'C36 H46 Cu Mo8 N12 O30'
_chemical_formula_weight         1957.91
_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                65.070(4)
_cell_angle_beta                 71.264(5)
_cell_angle_gamma                68.809(5)
_cell_formula_units_Z            1
_cell_length_a                   10.5513(7)
_cell_length_b                   12.9013(5)
_cell_length_c                   13.0406(6)
_cell_measurement_reflns_used    6037
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      26.3137
_cell_measurement_theta_min      2.9168
_cell_volume                     1470.67(15)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega  -76.00  -32.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.1323  128.0000  -36.0000 44

  2 omega  -19.00   12.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.1323  -99.0000 -180.0000 31

  3 omega   -4.00   62.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       19.6323  -99.0000  -90.0000 66

  4 omega   36.00   64.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       19.6323  178.0000   60.0000 28

  5 omega   -5.00   70.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       19.6323   37.0000 -150.0000 75

  6 omega  -53.00   64.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       19.6323  -19.0000    0.0000 117

  7 omega   -6.00   70.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       19.6323   37.0000   60.0000 76
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0603569000
_diffrn_orient_matrix_UB_12      -0.0065931000
_diffrn_orient_matrix_UB_13      0.0175368000
_diffrn_orient_matrix_UB_21      0.0348079000
_diffrn_orient_matrix_UB_22      0.0172778000
_diffrn_orient_matrix_UB_23      -0.0585496000
_diffrn_orient_matrix_UB_31      -0.0236567000
_diffrn_orient_matrix_UB_32      0.0600628000
_diffrn_orient_matrix_UB_33      -0.0033859000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0287
_diffrn_reflns_av_unetI/netI     0.0572
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12140
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.92
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.097
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97715
_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    2.211
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             951
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.754
_refine_diff_density_min         -0.648
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     400
_refine_ls_number_reflns         6016
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_gt           0.0325
_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^)+(0.0114P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0496
_refine_ls_wR_factor_ref         0.0541
_reflns_number_gt                4804
_reflns_number_total             6016
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce41223g.txt
_cod_data_source_block           nyy2013031803
_cod_original_cell_volume        1470.68(13)
_cod_database_code               7211342
_chemical_oxdiff_formula         C20H20N4O4Mo8Cu1
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  H16 of C16, {H15A,H15B} of C15, H14 of C14, H2 of C2, H13 of C13, H10 of
  C10, {H7A,H7B} of C7, H18 of C18, H12 of C12, H6 of N6, H17 of C17, {H11A,
  H11B} of C11, H8 of C8, H6A of C6, H9 of C9, H4 of C4
 At 1.5 times of:
  {H14A,H14B} of O14, {H15C,H15D} of O15
2.a Free rotating group:
 O14(H14A,H14B), O15(H15C,H15D)
2.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C11(H11A,H11B), C15(H15A,H15B)
2.c Aromatic/amide H refined with riding coordinates:
 N6(H6), C2(H2), C4(H4), C6(H6A), C8(H8), C9(H9), C10(H10), C12(H12), C13(H13),
  C14(H14), C16(H16), C17(H17), C18(H18)
;