Microwave assisted synthesis of a mono organoimido functionalized Anderson polyoxometalate.
Ritchie, C.; Bryant, G.; Dalton transactions (Cambridge, England : 2003) 44 (2015) 20826–20829; doi:10.1039/c5dt04000k

data_7037554
_publ_section_title
;
 Microwave assisted synthesis of a mono organoimido functionalized
 Anderson polyoxometalate.
;
_journal_issue                   48
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              20826
_journal_page_last               20829
_journal_paper_doi               10.1039/c5dt04000k
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         '2(C8 Mn Mo12 N2 O42), 10(C16 H36 N1)'
_chemical_formula_sum            'C176 H388 Mn2 Mo24 N12 O84'
_chemical_formula_weight         6429.40
_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'
_audit_creation_date             2015-10-19
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2015-10-22 deposited with the CCDC.
2015-11-10 downloaded from the CCDC.
;
_cell_angle_alpha                101.568(2)
_cell_angle_beta                 104.538(2)
_cell_angle_gamma                106.610(2)
_cell_formula_units_Z            2
_cell_length_a                   18.6267(4)
_cell_length_b                   26.5079(7)
_cell_length_c                   34.0911(10)
_cell_measurement_reflns_used    19868
_cell_measurement_temperature    130.00(10)
_cell_measurement_theta_max      76.7200
_cell_measurement_theta_min      3.4790
_cell_volume                     14925.9(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    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      130.00(10)
_diffrn_detector_area_resol_mean 10.2273
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_details
;
  1 omega -122.00   -5.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.8407  -77.0000 -180.0000 117

  2 omega  -48.00   40.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.8407   37.0000  -60.0000 88

  3 omega -130.00  -35.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -68.5000  -61.0000 -150.0000 95

  4 omega  -90.00    1.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -68.5000  111.0000  120.0000 91

  5 omega  -87.00   -5.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -68.5000  111.0000  -60.0000 82

  6 omega  -55.00   10.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -68.5000   45.0000   90.0000 65

  7 omega -142.00  -79.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -68.5000 -111.0000  -30.0000 63

  8 omega   29.00  108.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      116.0000  -94.0000   30.0000 79

  9 omega  101.00  177.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      116.0000  111.0000   60.0000 76

 10 omega   35.00  116.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      116.0000 -111.0000    0.0000 81

 11 omega  118.00  177.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      116.0000  111.0000 -180.0000 59

 12 omega   83.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      116.0000   61.0000  120.0000 95

 13 omega   74.00  108.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      116.0000  -94.0000 -180.0000 34

 14 omega   78.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      116.0000   30.0000 -120.0000 100

 15 omega   38.00  148.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      116.0000  -61.0000  120.0000 110

 16 omega   35.00  116.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      116.0000 -111.0000  -60.0000 81

 17 omega   82.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      116.0000   30.0000 -180.0000 96

 18 omega   37.00  116.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      116.0000 -111.0000  120.0000 79

 19 omega   42.00   69.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      116.0000  -94.0000 -180.0000 27
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0027432000
_diffrn_orient_matrix_UB_12      0.0344276000
_diffrn_orient_matrix_UB_13      0.0428817000
_diffrn_orient_matrix_UB_21      -0.0380480000
_diffrn_orient_matrix_UB_22      -0.0532832000
_diffrn_orient_matrix_UB_23      0.0103227000
_diffrn_orient_matrix_UB_31      0.0830350000
_diffrn_orient_matrix_UB_32      -0.0008008000
_diffrn_orient_matrix_UB_33      0.0209652000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0748
_diffrn_reflns_av_unetI/netI     0.0871
_diffrn_reflns_laue_measured_fraction_full 0.996
_diffrn_reflns_laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            125551
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.805
_diffrn_reflns_theta_min         2.858
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.156
_exptl_absorpt_correction_T_max  0.668
_exptl_absorpt_correction_T_min  0.101
_exptl_absorpt_correction_type   gaussian
_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)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.431
_exptl_crystal_description       Rod
_exptl_crystal_F_000             6516
_exptl_crystal_recrystallization_method
'Recrystallisation with vapor diffusion'
_exptl_crystal_size_max          0.5725
_exptl_crystal_size_mid          0.2193
_exptl_crystal_size_min          0.0581
_refine_diff_density_max         1.404
_refine_diff_density_min         -1.255
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.927
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1661
_refine_ls_number_reflns         61437
_refine_ls_number_restraints     107
_refine_ls_restrained_S_all      0.931
_refine_ls_R_factor_all          0.1544
_refine_ls_R_factor_gt           0.1042
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2994
_refine_ls_wR_factor_ref         0.3438
_reflns_Friedel_coverage         0.000
_reflns_number_gt                26845
_reflns_number_total             61437
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt04000k2.cif
_cod_data_source_block           cr_mo6_mn_microwave
_cod_original_cell_volume        14925.9(7)
_cod_database_code               7037554
_chemical_oxdiff_formula         'C176 H388 Mn2 Mo24 N12 O84'
_reflns_odcompleteness_completeness 98.46
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     75.12
_olex2_refinement_description
;
1. Restrained distances
 C88-C87
 1.5 with sigma of 0.02
 C96-C95
 1.5 with sigma of 0.02
 C35-C36
 1.5 with sigma of 0.02
 C59-C60
 1.5 with sigma of 0.02
 C58-C59
 1.5 with sigma of 0.02
 C52-C51
 1.5 with sigma of 0.02
 C50-C51
 1.5 with sigma of 0.02
 C49-C50
 1.5 with sigma of 0.02
 C33-C34
 1.5 with sigma of 0.02
 C74-C75
 1.5 with sigma of 0.02
 C76-C75
 1.5 with sigma of 0.02
 C65-C66
 1.5 with sigma of 0.02
 C67-C68
 1.5 with sigma of 0.02
 C66-C67
 1.5 with sigma of 0.02
 N5-C1
 1.5 with sigma of 0.02
 N5-C13
 1.5 with sigma of 0.02
 N5-C9
 1.5 with sigma of 0.02
 N5-C5
 1.5 with sigma of 0.02
 C9-C10
 1.5 with sigma of 0.02
 C10-C11
 1.5 with sigma of 0.02
 C5-C6
 1.5 with sigma of 0.02
 C1-C2
 1.5 with sigma of 0.02
 C2-C3
 1.5 with sigma of 0.02
 C4-C3
 1.5 with sigma of 0.02
 C12-C11
 1.5 with sigma of 0.02
 C8-C7
 1.5 with sigma of 0.02
 C7-C6
 1.5 with sigma of 0.02
 C126-C127
 1.5 with sigma of 0.02
 C113-C114
 1.5 with sigma of 0.02
 C114-C115
 1.5 with sigma of 0.02
 C116-C115
 1.5 with sigma of 0.02
 N12-C117
 1.5 with sigma of 0.02
 C117-C118
 1.5 with sigma of 0.02
 C118-C119
 1.5 with sigma of 0.02
 C119-C120
 1.5 with sigma of 0.02
 N9-C73
 1.5 with sigma of 0.02
 C73-C74
 1.5 with sigma of 0.02
 N6-C29
 1.5 with sigma of 0.02
 C29-C30
 1.5 with sigma of 0.02
 C30-C31
 1.5 with sigma of 0.02
 C31-C32
 1.5 with sigma of 0.02
 N6-C25
 1.5 with sigma of 0.02
 C26-C25
 1.5 with sigma of 0.02
 C21-N6
 1.5 with sigma of 0.02
 C22-C21
 1.5 with sigma of 0.02
 C22-C23
 1.5 with sigma of 0.02
 C17-N6
 1.5 with sigma of 0.02
 C18-C17
 1.5 with sigma of 0.02
 C19-C18
 1.5 with sigma of 0.02
 C20-C19
 1.5 with sigma of 0.02
 C24-C23
 1.5 with sigma of 0.02
 C34-C35
 1.5 with sigma of 0.02
 C36-C35
 1.5 with sigma of 0.02
 C86-C87
 1.5 with sigma of 0.02
 C88-C87
 1.5 with sigma of 0.02
 C13-C14
 1.5 with sigma of 0.02
 C14-C15
 1.5 with sigma of 0.02
 C15-C16
 1.5 with sigma of 0.02
 C99A-C127
 1.5 with sigma of 0.02
 C127-C99A
 1.5 with sigma of 0.02
 C99A-C127
 1.5 with sigma of 0.02
 C46-C47
 1.5 with sigma of 0.02
 C47-C47A
 1.5 with sigma of 0.02
 C45-C46
 1.5 with sigma of 0.02
 C46-C47
 1.5 with sigma of 0.02
 C46A-C45
 1.5 with sigma of 0.02
 C47A-C46A
 1.5 with sigma of 0.02
 C93A-N10
 1.6 with sigma of 0.02
 C93-N10
 1.6 with sigma of 0.02
 C94A-C93A
 1.5 with sigma of 0.02
 C94-C93
 1.5 with sigma of 0.02
 C94-C95
 1.5 with sigma of 0.02
 C94A-C95
 1.5 with sigma of 0.02
 C27-C28A
 1.5 with sigma of 0.02
 C28-C27
 1.5 with sigma of 0.02
 C86-C88
 2.1 with sigma of 0.04
 C86-C88
 2.65 with sigma of 0.04
 C34-C36
 2.65 with sigma of 0.04
 C58-C60
 2.65 with sigma of 0.04
 C50-C52
 2.65 with sigma of 0.04
 C74-C76
 2.65 with sigma of 0.04
 C66-C68
 2.65 with sigma of 0.04
 C1-C13
 2.65 with sigma of 0.04
 C113-C115
 2.65 with sigma of 0.04
 C116-C114
 2.65 with sigma of 0.04
 C113-C115
 2.65 with sigma of 0.04
 N12-C118
 2.65 with sigma of 0.04
 C117-C119
 2.65 with sigma of 0.04
 C117-C119
 2.65 with sigma of 0.04
 C120-C118
 2.65 with sigma of 0.04
 N9-C74
 2.65 with sigma of 0.04
 N6-C30
 2.65 with sigma of 0.04
 C29-C31
 2.65 with sigma of 0.04
 C30-C32
 2.65 with sigma of 0.04
 N6-C26
 2.65 with sigma of 0.04
 C29-C25
 2.65 with sigma of 0.04
 C29-C21
 2.65 with sigma of 0.04
 C25-C21
 2.65 with sigma of 0.04
 C23-C21
 2.65 with sigma of 0.04
 C17-C19
 2.65 with sigma of 0.04
 C18-C20
 2.65 with sigma of 0.04
 C24-C22
 2.65 with sigma of 0.04
 C17-C29
 2.5 with sigma of 0.04
 C86-C88
 2.5 with sigma of 0.04
 C13-C15
 2.55 with sigma of 0.04
 C99A-C126
 2.65 with sigma of 0.04
 C94-C96
 2.65 with sigma of 0.04
2. Uiso/Uaniso restraints and constraints
Uiso(C99A) = Uiso(C99A)
Uiso(C28A) = Uiso(C28)
3. Others
 Sof(C128)=1-FVAR(1)
 Sof(C99A)=FVAR(1)
 Sof(C80)=1-FVAR(2)
 Sof(C80A)=FVAR(2)
 Sof(C46A)=Sof(C47A)=1-FVAR(3)
 Sof(C46)=Sof(C47)=FVAR(3)
 Sof(C28)=1-FVAR(4)
 Sof(C28A)=FVAR(4)
 Sof(C93)=Sof(C94)=1-FVAR(5)
 Sof(C94A)=Sof(C93A)=FVAR(5)
 Fixed Sof: C24(0.5) C32(0.5) C84(0.5) C8(0.5) C68(0.5)
 Fixed Uiso: C29(0.18) C17(0.18) C18(0.18) C19(0.18) C20(0.18) C21(0.18)
 C22(0.18) C23(0.18) C24(0.18) C30(0.18) C31(0.18) C32(0.18) C25(0.18)
 C26(0.18) C27(0.18) C42(0.18) C43(0.18) C44(0.18) C39(0.18) C40(0.18)
 C35(0.18) C36(0.18) C94A(0.18) C93A(0.18) C89(0.17) C90(0.17) C91(0.17)
 C92(0.17) C84(0.17) C85(0.17) C86(0.17) C87(0.17) C88(0.18) C93(0.18)
 C94(0.18) C96(0.18) C121(0.18) C122(0.18) C123(0.18) C124(0.18) C125(0.18)
 C126(0.18) C127(0.18) C117(0.18) C118(0.18) C119(0.18) C120(0.18) C113(0.18)
 C114(0.18) C115(0.18) C116(0.18) N12(0.18) C8(0.18) C1(0.18) C2(0.18) C3(0.18)
 C5(0.18) C6(0.18) C7(0.18) C4(0.18) C14(0.18) C15(0.18) C16(0.18) C9(0.18)
 C10(0.18) C11(0.18) C12(0.18) N5(0.12) C66(0.18) C67(0.18) C68(0.18) C74(0.18)
 C75(0.18) C76(0.18) C58(0.18) C59(0.18) C60(0.18) C49(0.18) C50(0.18)
 C51(0.18) C52(0.18) C108(0.18)
;
_shelx_res_checksum              67920
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2014-12-22
_olex2_submission_special_instructions 'No special instructions were received'