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_7211345
_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         'C18 H18 Mo1 N6 O4 Zn1, 3(H2 O)'
_chemical_formula_sum            'C18 H24 Mo N6 O7 Zn'
_chemical_formula_weight         597.74
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      trigonal
_space_group_IT_number           147
_space_group_name_Hall           '-P 3'
_space_group_name_H-M_alt        'P -3'
_symmetry_space_group_name_Hall  '-P 3'
_symmetry_space_group_name_H-M   'P -3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-05-09
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   11.8441(5)
_cell_length_b                   11.8441(5)
_cell_length_c                   9.2064(4)
_cell_measurement_reflns_used    1106
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      26.2090
_cell_measurement_theta_min      3.9690
_cell_volume                     1118.47(8)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega  -21.00   54.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7885  -99.0000    0.0000 75

  2 omega   34.00   73.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7885 -178.0000  150.0000 39
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0582784000
_diffrn_orient_matrix_UB_12      -0.0031167000
_diffrn_orient_matrix_UB_13      -0.0004740000
_diffrn_orient_matrix_UB_21      -0.0343734000
_diffrn_orient_matrix_UB_22      -0.0641009000
_diffrn_orient_matrix_UB_23      0.0285610000
_diffrn_orient_matrix_UB_31      -0.0140627000
_diffrn_orient_matrix_UB_32      -0.0255446000
_diffrn_orient_matrix_UB_33      -0.0716331000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0191
_diffrn_reflns_av_unetI/netI     0.0412
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            2458
_diffrn_reflns_theta_full        26.36
_diffrn_reflns_theta_max         26.36
_diffrn_reflns_theta_min         2.97
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.686
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97394
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.775
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             604
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.716
_refine_diff_density_min         -0.703
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     100
_refine_ls_number_reflns         1542
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0651
_refine_ls_R_factor_gt           0.0489
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1428
_refine_ls_wR_factor_ref         0.1576
_reflns_number_gt                1211
_reflns_number_total             1542
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce41223g.txt
_cod_data_source_block           nyy13050701
_cod_database_code               7211345
_chemical_oxdiff_formula         C20H20N4O4Mo1
_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:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Mo1 \\sim O1: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
3.a Riding coordinates:
 O3(H3A,H3B)
3.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B)
3.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C6(H6)
;