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_7221903
_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         'C42 H52 Mo12 N12 O38, 4(O)'
_chemical_formula_sum            'C42 H60 Mo12 N12 O42'
_chemical_formula_weight         2556.30
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-06-30
_audit_creation_method
;
Olex2 1.2
(compiled 2014.06.26 svn.r2951 for OlexSys, GUI svn.r4855)
;
_audit_update_record
;
2015-04-01 deposited with the CCDC.
2015-08-26 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.9997(3)
_cell_length_b                   14.97489(18)
_cell_length_c                   25.4844(5)
_cell_measurement_reflns_used    8616
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      28.7430
_cell_measurement_theta_min      3.3300
_cell_volume                     7250.8(2)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega   43.00   68.65   0.4500   11.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7104   77.0000   60.0000 57

  2 omega   45.00   88.20   0.4500   11.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7104   77.0000 -120.0000 96

  3 omega   51.00   76.65   0.4500   11.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7104   77.0000 -180.0000 57

  4 omega    1.00   49.15   0.4500   11.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7104   77.0000   90.0000 107

  5 omega  -10.00   28.25   0.4500   11.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7104   77.0000   60.0000 85
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0367647000
_diffrn_orient_matrix_UB_12      0.0017664000
_diffrn_orient_matrix_UB_13      0.0047876000
_diffrn_orient_matrix_UB_21      0.0059956000
_diffrn_orient_matrix_UB_22      0.0096265000
_diffrn_orient_matrix_UB_23      -0.0268815000
_diffrn_orient_matrix_UB_31      -0.0026535000
_diffrn_orient_matrix_UB_32      0.0463212000
_diffrn_orient_matrix_UB_33      0.0054152000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0353
_diffrn_reflns_av_unetI/netI     0.0405
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            23355
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.96
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.103
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95046
_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    2.342
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4944
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.905
_refine_diff_density_min         -0.653
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     503
_refine_ls_number_reflns         7406
_refine_ls_number_restraints     29
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0659
_refine_ls_R_factor_gt           0.0468
_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^)+(0.0327P)^2^+36.1011P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0971
_refine_ls_wR_factor_ref         0.1056
_reflns_number_gt                5838
_reflns_number_total             7406
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ra13007g2.cif
_cod_data_source_block           exp_8320
_cod_database_code               7221903
_chemical_oxdiff_formula         C20H20N4O4Mo1
_reflns_odcompleteness_completeness 99.73
_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
2. Restrained distances
 C20-C19
 1.4 with sigma of 0.02
 N5-C19
 1.4 with sigma of 0.02
 N6-C20
 1.4 with sigma of 0.02
 C21-N6
 1.4 with sigma of 0.02
 C21-N5
 1.4 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C21) \\sim Ueq, Uanis(N6) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C19)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O20) = Uanis(O20A)
4. Others
 Sof(O20A)=1-FVAR(1)
 Sof(O20)=FVAR(1)
 Fixed Sof: O21(0.5) O22(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C9(H9A,H9B), C11(H11A,H11B)
5.b Aromatic/amide H refined with riding coordinates:
 N4(H4), N6(H6), C13(H13), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18),
 C19(H19), C20(H20), C21(H21)
5.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C)
;
_olex2_submission_special_instructions 'No special instructions were received'