A cyanide-bridged wheel featuring a seven-coordinate Mo(III) center
Kempe, David Kenneth; Dolinar, Brian; Vignesh, Kuduva R.; Woods, Toby; Saber, Mohamed R.; Dunbar, Kim R.; Chemical Communications  (2019) –; doi:10.1039/C8CC09373C

data_7122875
_publ_section_title
;
 A cyanide-bridged wheel featuring a seven-coordinate Mo(III) center
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C8CC09373C
_journal_year                    2019
_chemical_formula_moiety         'C222 H276 Mo6 N90 Ni12 O6'
_chemical_formula_sum            'C222 H276 Mo6 N90 Ni12 O6'
_chemical_formula_weight         5581.47
_chemical_properties_physical    Air-sensitive
_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
_audit_creation_date             2018-04-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.18 svn.r3501 for OlexSys, GUI svn.r5488)
;
_audit_update_record
;
2018-06-25 deposited with the CCDC.
2019-01-17 downloaded from the CCDC.
;
_cell_angle_alpha                105.168(3)
_cell_angle_beta                 105.407(2)
_cell_angle_gamma                104.914(2)
_cell_formula_units_Z            1
_cell_length_a                   20.8632(17)
_cell_length_b                   20.9777(19)
_cell_length_c                   21.0033(18)
_cell_measurement_reflns_used    9897
_cell_measurement_temperature    110.0
_cell_measurement_theta_max      24.256
_cell_measurement_theta_min      2.455
_cell_volume                     8008.1(12)
_computing_cell_refinement       'SAINT+ Ver. 8.34A (Bruker-AXS, 2014)'
_computing_data_collection       'APEX3(Bruker-AXS, 2015)'
_computing_data_reduction        'SAINT+ Ver. 8.34A (Bruker-AXS, 2014)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008-2013)'
_diffrn_ambient_temperature      110.0
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker PHOTON area detector'
_diffrn_measurement_method       '0.5\ \w and 0.5\ \f scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0848
_diffrn_reflns_av_unetI/netI     0.0814
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            89054
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        24.301
_diffrn_reflns_theta_max         24.301
_diffrn_reflns_theta_min         2.034
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.968
_exptl_absorpt_correction_T_max  0.6458
_exptl_absorpt_correction_T_min  0.4828
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1244 before and 0.0667 after correction. The Ratio of minimum to maximum transmission is 0.7476. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.157
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2874
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.959
_refine_diff_density_min         -1.009
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2122
_refine_ls_number_reflns         25768
_refine_ls_number_restraints     2764
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.1361
_refine_ls_R_factor_gt           0.0881
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0497P)^2^+87.2994P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1838
_refine_ls_wR_factor_ref         0.2110
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16727
_reflns_number_total             25768
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc09373c2.cif
_cod_data_source_block           dkk2_310_0m_sq
_cod_original_cell_volume        8008.0(12)
_cod_database_code               7122875
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.953
_shelx_estimated_absorpt_t_min   0.643
_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. Restrained distances
 O1-H1B = O1-H1A = O3-H3B = O3-H3A = O2-H2A = O2-H2B = O2A-H2AA = O2A-H2AB
 0.84 with sigma of 0.01
 H1B-H1A = H3B-H3A = H2A-H2B = H2AA-H2AB
 1.33 with sigma of 0.01
 N45-C111 \\sim N45A-C1A \\sim N31-C97 \\sim N31A-C97A
 with sigma of 0.01
 Ni4-N14 \\sim Ni4A-N14A
 with sigma of 0.01
 Ni4-O2 \\sim Ni4A-O2A
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
N5 \\sim N6 \\sim N7 \\sim N8 \\sim C16 \\sim C17 \\sim C18 \\sim C19 \\sim C20
\\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25 \\sim C26 \\sim C27 \\sim C28
\\sim C29 \\sim C30 \\sim N13 \\sim N14 \\sim N15 \\sim N16 \\sim C46 \\sim C47
\\sim C48 \\sim C49 \\sim C50 \\sim C51 \\sim C52 \\sim C53 \\sim C54 \\sim C55
\\sim C56 \\sim C57 \\sim C58 \\sim C59 \\sim C60 \\sim N21 \\sim N22 \\sim N23
\\sim N24 \\sim C76 \\sim C77 \\sim C78 \\sim C79 \\sim C80 \\sim C81 \\sim C82
\\sim C83 \\sim C84 \\sim C85 \\sim C86 \\sim C87 \\sim C88 \\sim C89 \\sim C90
\\sim N5A \\sim N6A \\sim N7A \\sim N8A \\sim C16A \\sim C17A \\sim C18A \\sim
C19A \\sim C20A \\sim C21A \\sim C22A \\sim C23A \\sim C24A \\sim C25A \\sim
C26A \\sim C27A \\sim C28A \\sim C29A \\sim C30A \\sim N13A \\sim N14A \\sim
N15A \\sim N16A \\sim C46A \\sim C47A \\sim C48A \\sim C49A \\sim C50A \\sim
C51A \\sim C52A \\sim C53A \\sim C54A \\sim C55A \\sim C56A \\sim C57A \\sim
C58A \\sim C59A \\sim C60A \\sim N21A \\sim N22A \\sim N23A \\sim N24A \\sim
C76A \\sim C77A \\sim C78A \\sim C79A \\sim C80A \\sim C81A \\sim C82A \\sim
C83A \\sim C84A \\sim C85A \\sim C86A \\sim C87A \\sim C88A \\sim C89A \\sim
C90A: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
N36A \\sim C1B \\sim C102 \\sim N36: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.02
C1A \\sim N45A \\sim C111 \\sim N45: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.02
C97 \\sim C97A \\sim N31A \\sim N31: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.02
O2A \\sim O2 \\sim Ni4 \\sim Ni4A: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O2A) = Uanis(O2)
4. Same fragment restrains
{N5, N6, N7, N8, C16, C17, C18, C19, C20, C21, C22, C23, C24, C25, C26, C27,
C28, C29, C30} sigma for 1-2: 0.005, 1-3: 0.01
{N5A, N6A, N7A, N8A, C16A, C17A, C18A, C19A, C20A, C21A, C22A, C23A, C24A,
C25A, C26A, C27A, C28A, C29A, C30A} sigma for 1-2: 0.005, 1-3: 0.01
{N13, N14, N15, N16, C46, C47, C48, C49, C50, C51, C52, C53, C54, C55, C56,
C57, C58, C59, C60} sigma for 1-2: 0.005, 1-3: 0.01
{N13A, N14A, N15A, N16A, C46A, C47A, C48A, C49A, C50A, C51A, C52A, C53A, C54A,
C55A, C56A, C57A, C58A, C59A, C60A} sigma for 1-2: 0.005, 1-3: 0.01
{N21, N22, N23, N24, C76, C77, C78, C79, C80, C81, C82, C83, C84, C85, C86,
C87, C88, C89, C90} sigma for 1-2: 0.005, 1-3: 0.01
{N21A, N22A, N23A, N24A, C76A, C77A, C78A, C79A, C80A, C81A, C82A, C83A, C84A,
C85A, C86A, C87A, C88A, C89A, C90A} sigma for 1-2: 0.005, 1-3: 0.01
as
{N1, N2, N3, N4, C1, C2, C3, C4, C5, C6, C7, C8, C9, C10, C11, C12, C13, C14,
C15}
5. Others
 Sof(N21A)=Sof(N22A)=Sof(N23A)=Sof(H23E)=Sof(N24A)=Sof(C76A)=Sof(H76A)=
 Sof(C77A)=Sof(H77A)=Sof(C78A)=Sof(C79A)=Sof(C80A)=Sof(H80D)=Sof(H80E)=
 Sof(H80F)=Sof(C81A)=Sof(H81C)=Sof(H81D)=Sof(C82A)=Sof(H82C)=Sof(H82D)=
 Sof(C83A)=Sof(H83C)=Sof(H83D)=Sof(C84A)=Sof(H84C)=Sof(H84D)=Sof(C85A)=
 Sof(H85C)=Sof(H85D)=Sof(C86A)=Sof(H86C)=Sof(H86D)=Sof(C87A)=Sof(C88A)=
 Sof(H88D)=Sof(H88E)=Sof(H88F)=Sof(C89A)=Sof(C90A)=Sof(H90A)=1-FVAR(1)
 Sof(N21)=Sof(N22)=Sof(N23)=Sof(H23)=Sof(N24)=Sof(C76)=Sof(H76)=Sof(C77)=
 Sof(H77)=Sof(C78)=Sof(C79)=Sof(C80)=Sof(H80A)=Sof(H80B)=Sof(H80C)=Sof(C81)=
 Sof(H81A)=Sof(H81B)=Sof(C82)=Sof(H82A)=Sof(H82B)=Sof(C83)=Sof(H83A)=Sof(H83B)=
 Sof(C84)=Sof(H84A)=Sof(H84B)=Sof(C85)=Sof(H85A)=Sof(H85B)=Sof(C86)=Sof(H86A)=
 Sof(H86B)=Sof(C87)=Sof(C88)=Sof(H88A)=Sof(H88B)=Sof(H88C)=Sof(C89)=Sof(C90)=
 Sof(H90)=FVAR(1)
 Sof(N13A)=Sof(N14A)=Sof(N15A)=Sof(H15B)=Sof(N16A)=Sof(C46A)=Sof(H46A)=
 Sof(C47A)=Sof(H47A)=Sof(C48A)=Sof(C49A)=Sof(C50A)=Sof(H50D)=Sof(H50E)=
 Sof(H50F)=Sof(C51A)=Sof(H51C)=Sof(H51D)=Sof(C52A)=Sof(H52C)=Sof(H52D)=
 Sof(C53A)=Sof(H53C)=Sof(H53D)=Sof(C54A)=Sof(H54C)=Sof(H54D)=Sof(C55A)=
 Sof(H55C)=Sof(H55D)=Sof(C56A)=Sof(H56C)=Sof(H56D)=Sof(C57A)=Sof(C58A)=
 Sof(H58D)=Sof(H58E)=Sof(H58F)=Sof(C59A)=Sof(C60A)=Sof(H60A)=Sof(O2A)=Sof(H2AA)=
 Sof(H2AB)=Sof(Ni4A)=1-FVAR(2)
 Sof(Ni4)=Sof(O2)=Sof(H2A)=Sof(H2B)=Sof(N13)=Sof(N14)=Sof(N15)=Sof(H15A)=
 Sof(N16)=Sof(C46)=Sof(H46)=Sof(C47)=Sof(H47)=Sof(C48)=Sof(C49)=Sof(C50)=
 Sof(H50A)=Sof(H50B)=Sof(H50C)=Sof(C51)=Sof(H51A)=Sof(H51B)=Sof(C52)=Sof(H52A)=
 Sof(H52B)=Sof(C53)=Sof(H53A)=Sof(H53B)=Sof(C54)=Sof(H54A)=Sof(H54B)=Sof(C55)=
 Sof(H55A)=Sof(H55B)=Sof(C56)=Sof(H56A)=Sof(H56B)=Sof(C57)=Sof(C58)=Sof(H58A)=
 Sof(H58B)=Sof(H58C)=Sof(C59)=Sof(C60)=Sof(H60)=FVAR(2)
 Sof(N5A)=Sof(N6A)=Sof(N7A)=Sof(H7AA)=Sof(N8A)=Sof(C16A)=Sof(H16A)=Sof(C17A)=
 Sof(H17A)=Sof(C18A)=Sof(C19A)=Sof(C20A)=Sof(H20D)=Sof(H20E)=Sof(H20F)=
 Sof(C21A)=Sof(H21C)=Sof(H21D)=Sof(C22A)=Sof(H22C)=Sof(H22D)=Sof(C23A)=
 Sof(H23C)=Sof(H23D)=Sof(C24A)=Sof(H24C)=Sof(H24D)=Sof(C25A)=Sof(H25C)=
 Sof(H25D)=Sof(C26A)=Sof(H26C)=Sof(H26D)=Sof(C27A)=Sof(C28A)=Sof(H28D)=
 Sof(H28E)=Sof(H28F)=Sof(C29A)=Sof(C30A)=Sof(H30A)=1-FVAR(3)
 Sof(N5)=Sof(N6)=Sof(N7)=Sof(H7)=Sof(N8)=Sof(C16)=Sof(H16)=Sof(C17)=Sof(H17)=
 Sof(C18)=Sof(C19)=Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(H20C)=Sof(C21)=Sof(H21A)=
 Sof(H21B)=Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(C24)=
 Sof(H24A)=Sof(H24B)=Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(C26)=Sof(H26A)=Sof(H26B)=
 Sof(C27)=Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(H28C)=Sof(C29)=Sof(C30)=Sof(H30)=
 FVAR(3)
 Sof(C97A)=Sof(N31A)=1-FVAR(4)
 Sof(N31)=Sof(C97)=FVAR(4)
 Sof(N45A)=Sof(C1A)=1-FVAR(5)
 Sof(N45)=Sof(C111)=FVAR(5)
 Sof(C1B)=Sof(N36A)=1-FVAR(6)
 Sof(N36)=Sof(C102)=FVAR(6)
6.a Ternary CH refined with riding coordinates:
 N11(H11), N19(H19), N3(H3), N7(H7), N15(H15A), N23(H23), N7A(H7AA),
 N15A(H15B), N23A(H23E)
6.b Secondary CH2 refined with riding coordinates:
 C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B), C40(H40A,
 H40B), C41(H41A,H41B), C66(H66A,H66B), C67(H67A,H67B), C68(H68A,H68B),
 C69(H69A,H69B), C70(H70A,H70B), C71(H71A,H71B), C6(H6A,H6B), C7(H7A,H7B),
 C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C21(H21A,H21B),
 C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B),
  C51(H51A,H51B), C52(H52A,H52B), C53(H53A,H53B), C54(H54A,H54B), C55(H55A,
 H55B), C56(H56A,H56B), C81(H81A,H81B), C82(H82A,H82B), C83(H83A,H83B),
 C84(H84A,H84B), C85(H85A,H85B), C86(H86A,H86B), C21A(H21C,H21D), C22A(H22C,
 H22D), C23A(H23C,H23D), C24A(H24C,H24D), C25A(H25C,H25D), C26A(H26C,H26D),
 C51A(H51C,H51D), C52A(H52C,H52D), C53A(H53C,H53D), C54A(H54C,H54D), C55A(H55C,
 H55D), C56A(H56C,H56D), C81A(H81C,H81D), C82A(H82C,H82D), C83A(H83C,H83D),
 C84A(H84C,H84D), C85A(H85C,H85D), C86A(H86C,H86D)
6.c Aromatic/amide H refined with riding coordinates:
 C31(H31), C32(H32), C45(H45), C61(H61), C62(H62), C75(H75), C1(H1), C2(H2),
 C15(H15), C16(H16), C17(H17), C30(H30), C46(H46), C47(H47), C60(H60), C76(H76),
  C77(H77), C90(H90), C16A(H16A), C17A(H17A), C30A(H30A), C46A(H46A),
 C47A(H47A), C60A(H60A), C76A(H76A), C77A(H77A), C90A(H90A)
6.d Idealised Me refined with riding coordinates:
 C35(H35A,H35B,H35C), C43(H43A,H43B,H43C), C65(H65A,H65B,H65C), C73(H73A,H73B,
 H73C), C5(H5A,H5B,H5C), C13(H13A,H13B,H13C), C20(H20A,H20B,H20C), C28(H28A,
 H28B,H28C), C50(H50A,H50B,H50C), C58(H58A,H58B,H58C), C80(H80A,H80B,H80C),
 C88(H88A,H88B,H88C), C20A(H20D,H20E,H20F), C28A(H28D,H28E,H28F), C50A(H50D,
 H50E,H50F), C58A(H58D,H58E,H58F), C80A(H80D,H80E,H80F), C88A(H88D,H88E,H88F)
;
_shelx_res_checksum              25657
_shelx_hkl_checksum              54504
_shelx_fab_checksum              5607
_olex2_submission_special_instructions 'No special instructions were received'