Phosphorescent complexes of {Mo6I8}4+ with triazolates: [2+3] cycloaddition of alkynes to [Mo6I8(N3)6]2−
Mironova, Alina D.; Mikhailov, Maksim A.; Brylev, Konstantin A.; Gushchin, Artem L.; Sukhikh, Taisiya S.; Sokolov, Maxim N.; New Journal of Chemistry 44 (2020) 20620–20625; doi:10.1039/D0NJ04259E

data_7060028
_publ_section_title
;
 Phosphorescent complexes of {Mo6I8}4+ with triazolates: [2+3]
 cycloaddition of alkynes to [Mo6I8(N3)6]2&#x2212;
;
_journal_issue                   47
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              20620
_journal_page_last               20625
_journal_paper_doi               10.1039/D0NJ04259E
_journal_volume                  44
_journal_year                    2020
_chemical_formula_moiety         'C36 H36 I8 Mo6 N18 O24, 2(C16 H36 N)'
_chemical_formula_sum            'C68 H108 I8 Mo6 N20 O24'
_chemical_formula_weight         3180.58
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-03-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-03-21 deposited with the CCDC.	2020-10-06 downloaded from the CCDC.
;
_cell_angle_alpha                92.521(4)
_cell_angle_beta                 110.391(4)
_cell_angle_gamma                113.893(4)
_cell_formula_units_Z            1
_cell_length_a                   12.9853(14)
_cell_length_b                   15.2882(17)
_cell_length_c                   15.6326(16)
_cell_measurement_reflns_used    9242
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      28.64
_cell_measurement_theta_min      2.54
_cell_volume                     2596.9(5)
_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      298(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0338
_diffrn_reflns_av_unetI/netI     0.0415
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            29056
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_min         1.492
_exptl_absorpt_coefficient_mu    3.152
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.5992
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.0720 before and 0.0480 after correction. The Ratio of minimum to maximum transmission is 0.8032. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.034
_exptl_crystal_description       prism
_exptl_crystal_F_000             1524
_exptl_crystal_preparation       Luminescent
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.123
_refine_diff_density_min         -0.625
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     644
_refine_ls_number_reflns         9830
_refine_ls_number_restraints     252
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0581
_refine_ls_R_factor_gt           0.0347
_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^)+(0.0421P)^2^+1.7551P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0815
_refine_ls_wR_factor_ref         0.0948
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6999
_reflns_number_total             9830
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj04259e2.cif
_cod_data_source_block           amd144
_cod_depositor_comments          'Adding full bibliography for 7060028.cif.'
_cod_database_code               7060028
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.743
_shelx_estimated_absorpt_t_min   0.405
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C63B-C62 = C63A-C62 = C63A-C64A = C63B-C64B
 1.55 with sigma of 0.02
 C71-C72A = C71-C72B = C73A-C72A = C73B-C72B = C74A-C73A = C74B-C73B
 1.55 with sigma of 0.02
 C25A-C22 \\sim C22-C25B
 with sigma of 0.02
 O23A-C25A \\sim O23B-C25B
 with sigma of 0.02
 O24A-C25A \\sim O24B-C25B
 with sigma of 0.02
 O23A-O24A \\sim O23B-O24B
 with sigma of 0.02
 C23A-C21 \\sim C23B-C21
 with sigma of 0.02
 O21A-C23A \\sim O21B-C23B
 with sigma of 0.02
 O22A-C23A \\sim O22B-C23B
 with sigma of 0.02
 O22A-C24A \\sim O22B-C24B
 with sigma of 0.02
 C23A-C24A \\sim C23B-C24B
 with sigma of 0.02
 O24A-C26A \\sim O24B-C26B
 with sigma of 0.02
3. Restrained planarity
 C21, O21B, O22B, C23B
 with sigma of 0.1
 C21, O21A, O22A, C23A
 with sigma of 0.1
4. Rigid bond restraints
 O21A, O22A, C23A, C24A, O21B, O22B, C23B, C24B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O23A, O24A, C25A, C26A, O23B, O24B, C25B, C26B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Uiso/Uaniso restraints and constraints
O21A \\sim O22A \\sim C23A \\sim C24A \\sim O21B \\sim O22B \\sim C23B \\sim
C24B: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
O23A \\sim O24A \\sim C25A \\sim C26A \\sim O23B \\sim O24B \\sim C25B \\sim
C26B: within 2A with sigma of 0.004 and sigma for terminal atoms of 0.008
Uiso(C63B) = Uiso(C63A) = Uiso(C64B) = Uiso(C64A)
Uiso(C72A) = Uiso(C72B) = Uiso(C73A) = Uiso(C73B) = Uiso(C74B) = Uiso(C74A)
6. Others
 Sof(O23B)=Sof(O24B)=Sof(C25B)=Sof(C26B)=Sof(H26D)=Sof(H26E)=Sof(H26F)=1-FVAR(1)
 Sof(O23A)=Sof(O24A)=Sof(C25A)=Sof(C26A)=Sof(H26A)=Sof(H26B)=Sof(H26C)=FVAR(1)
 Sof(O21B)=Sof(O22B)=Sof(C23B)=Sof(C24B)=Sof(H24D)=Sof(H24E)=Sof(H24F)=1-FVAR(2)
 Sof(O21A)=Sof(O22A)=Sof(C23A)=Sof(C24A)=Sof(H24A)=Sof(H24B)=Sof(H24C)=FVAR(2)
 Sof(H62C)=Sof(H62D)=Sof(C63B)=Sof(H63C)=Sof(H63D)=Sof(C64B)=Sof(H64D)=
 Sof(H64E)=Sof(H64F)=1-FVAR(3)
 Sof(H62A)=Sof(H62B)=Sof(C63A)=Sof(H63A)=Sof(H63B)=Sof(C64A)=Sof(H64A)=
 Sof(H64B)=Sof(H64C)=FVAR(3)
 Sof(H71C)=Sof(H71D)=Sof(C72B)=Sof(H72C)=Sof(H72D)=Sof(C73B)=Sof(H73C)=
 Sof(H73D)=Sof(C74B)=Sof(H74D)=Sof(H74E)=Sof(H74F)=1-FVAR(4)
 Sof(H71A)=Sof(H71B)=Sof(C72A)=Sof(H72A)=Sof(H72B)=Sof(C73A)=Sof(H73A)=
 Sof(H73B)=Sof(C74A)=Sof(H74A)=Sof(H74B)=Sof(H74C)=FVAR(4)
7.a Secondary CH2 refined with riding coordinates:
 C41(H41A,H41B), C42(H42A,H42B), C43(H43A,H43B), C51(H51A,H51B), C52(H52A,
 H52B), C53(H53A,H53B), C61(H61A,H61B), C62(H62C,H62D), C62(H62A,H62B),
 C71(H71A,H71B), C71(H71C,H71D), C63A(H63A,H63B), C72A(H72A,H72B), C73A(H73A,
 H73B), C63B(H63C,H63D), C72B(H72C,H72D), C73B(H73C,H73D)
7.b Idealised Me refined with riding coordinates:
 C24B(H24D,H24E,H24F)
7.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C34(H34A,H34B,H34C), C36(H36A,H36B,
 H36C), C24A(H24A,H24B,H24C), C26A(H26A,H26B,H26C), C26B(H26D,H26E,H26F),
 C44(H44A,H44B,H44C), C54(H54A,H54B,H54C), C64A(H64A,H64B,H64C), C74A(H74A,H74B,
 H74C), C64B(H64D,H64E,H64F), C74B(H74D,H74E,H74F)
;
_shelx_res_checksum              88564
_olex2_submission_special_instructions 'No special instructions were received'