Four hybrid compounds based on new type of molybdates and a flexible tripodal ligand: synthesis, structures, photochemical and electrochemical properties
Du, Hai-Juan; Wang, Chao-Hai; Li, Yao; Niu, Yunyin; Hou, Hongwei; RSC Adv.  (2015) –; doi:10.1039/C5RA13007G

data_7221906
_publ_section_title
;
 Four hybrid compounds based on new type of molybdates and a flexible
 tripodal ligand: synthesis, structures, photochemical and electrochemical
 properties
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C5RA13007G
_journal_year                    2015
_chemical_formula_moiety
'Mo8 O26, Co H4 Mo8 O28, 4.5(H2 O), 2(C21 H27 N6)'
_chemical_formula_sum            'C42 H67 Co Mo16 N12 O58.5'
_chemical_formula_weight         3270.04
_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   mixed
_atom_sites_solution_primary     heavy
_audit_creation_date             2015-04-01
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-04-01 deposited with the CCDC.
2015-08-26 downloaded from the CCDC.
;
_cell_angle_alpha                100.614(4)
_cell_angle_beta                 96.093(4)
_cell_angle_gamma                103.887(4)
_cell_formula_units_Z            1
_cell_length_a                   10.7586(5)
_cell_length_b                   11.3075(4)
_cell_length_c                   17.9670(9)
_cell_measurement_reflns_used    8209
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      28.9890
_cell_measurement_theta_min      3.2380
_cell_volume                     2059.49(17)
_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    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_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   28.00   53.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.1323   77.0000  -90.0000 25

  2 omega  -45.00   45.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.1323   77.0000   30.0000 90

  3 omega  -10.00   83.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7104   77.0000  150.0000 93

  4 omega    4.00   66.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7104   77.0000    0.0000 62

  5 omega   64.00   90.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7104   77.0000 -180.0000 26

  6 omega   -8.00   88.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7104   77.0000  -90.0000 96

  7 omega   32.00   80.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7104 -178.0000  -30.0000 48
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0364760000
_diffrn_orient_matrix_UB_12      0.0563889000
_diffrn_orient_matrix_UB_13      0.0253626000
_diffrn_orient_matrix_UB_21      0.0503258000
_diffrn_orient_matrix_UB_22      -0.0284449000
_diffrn_orient_matrix_UB_23      0.0083249000
_diffrn_orient_matrix_UB_31      0.0294364000
_diffrn_orient_matrix_UB_32      0.0198305000
_diffrn_orient_matrix_UB_33      -0.0306877000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0303
_diffrn_reflns_av_unetI/netI     0.0484
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            17103
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.030
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.655
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91272
_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    2.637
_exptl_crystal_F_000             1570
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.599
_refine_diff_density_min         -1.462
_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     599
_refine_ls_number_reflns         8405
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0437
_refine_ls_R_factor_gt           0.0329
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0246P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0648
_refine_ls_wR_factor_ref         0.0694
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7032
_reflns_number_total             8405
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ra13007g2.cif
_cod_data_source_block           nyy14060304
_cod_original_cell_volume        2059.51(16)
_cod_original_formula_sum        'C42 H67 Co Mo16 N12 O58.50'
_cod_database_code               7221906
_chemical_oxdiff_formula         C1H1O1N1Cl2Cd1Mo1
_shelx_estimated_absorpt_t_max   0.708
_shelx_estimated_absorpt_t_min   0.647
_reflns_odcompleteness_completeness 99.83
_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 C(H,H,H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O30) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Fixed Sof: O30(0.25) H30A(0.25) H30B(0.25)
4.a Riding coordinates:
 O30(H30A,H30B), O29(H29A,H29B)
4.b Free rotating group:
 O28(H28A,H28B)
4.c Rotating group:
 O27(H27A,H27B)
4.d Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C9(H9A,H9B), C11(H11A,H11B)
4.e Aromatic/amide H refined with riding coordinates:
 N2(H2), N4(H4), N6(H6), C13(H13), C14(H14), C15(H15), C16(H16), C17(H17),
 C18(H18), C19(H19), C20(H20), C21(H21)
4.f Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C)
;
_shelx_res_checksum              19938
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'