Discrete and polymeric ensembles based on dinuclear molybdenum(vi) building blocks with adaptive carbohydrazide ligands: from the design to catalytic epoxidation
Topić, Edi; Pisk, Jana; Agustin, Dominique; Jendrlin, Martin; Cvijanović, Danijela; Vrdoljak, Višnja; Rubčić, Mirta; New Journal of Chemistry 44 (2020) 8085–8097; doi:10.1039/D0NJ01045F

data_7059538
_publ_section_title
;
 Discrete and polymeric ensembles based on dinuclear molybdenum(vi)
 building blocks with adaptive carbohydrazide ligands: from the design to
 catalytic epoxidation
;
_journal_issue                   19
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              8085
_journal_page_last               8097
_journal_paper_doi               10.1039/D0NJ01045F
_journal_volume                  44
_journal_year                    2020
_chemical_formula_moiety         'C23 H22 Mo2 N8 O9, C2 H3 N'
_chemical_formula_sum            'C25 H25 Mo2 N9 O9'
_chemical_formula_weight         787.42
_chemical_name_systematic
;
2,2'-(carbonylbis(hydrazin-2-yl-1-ylidenemethylylidene))
di(3-methoxyphenolato))bis(imidazol)tetraoxo-di-molybdenum(vi)
acetonitrile solvate
;
_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   mixed
_audit_creation_date             2019-07-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-02-10 deposited with the CCDC.	2020-04-27 downloaded from the CCDC.
;
_cell_angle_alpha                85.958(3)
_cell_angle_beta                 87.645(3)
_cell_angle_gamma                81.166(3)
_cell_formula_units_Z            2
_cell_length_a                   8.2715(3)
_cell_length_b                   12.1751(5)
_cell_length_c                   15.0901(5)
_cell_measurement_reflns_used    7022
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.5500
_cell_measurement_theta_min      2.1920
_cell_volume                     1497.20(10)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150.15
_diffrn_detector_area_resol_mean 16.3426
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.877
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0315
_diffrn_reflns_av_unetI/netI     0.0513
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.877
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            18418
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.877
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.855
_diffrn_reflns_theta_min         2.100
_exptl_absorpt_coefficient_mu    0.905
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85353
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark orange'
_exptl_crystal_density_diffrn    1.747
_exptl_crystal_description       plate
_exptl_crystal_F_000             788
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.296
_refine_diff_density_min         -0.809
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     437
_refine_ls_number_reflns         9788
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0508
_refine_ls_R_factor_gt           0.0344
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0277P)^2^+0.6461P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0723
_refine_ls_wR_factor_ref         0.0803
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7752
_reflns_number_total             9788
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj01045f2.cif
_cod_data_source_block           5b_CH3CN
_cod_depositor_comments
;Adding full bibliography for 7059536--7059543.cif.

 Adding full bibliography for 7059536--7059543.cif.
;
_cod_database_code               7059538
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.915
_shelx_estimated_absorpt_t_min   0.714
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 H8-N8
 0.88 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(N5) = Uanis(C18B)
Uanis(C18B) = Uanis(N6B)
4. Others
 Sof(C18B)=Sof(H18B)=Sof(N6B)=Sof(H6B)=Sof(C19B)=Sof(H19B)=Sof(C20B)=Sof(H20B)=
 1-FVAR(1)
 Sof(N6A)=Sof(H6A)=Sof(C20A)=Sof(H20A)=Sof(C19A)=Sof(H19A)=Sof(C18A)=Sof(H18A)=
 FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C21(H21), C23(H23), C9(H9), C6(H6), C22(H22), C13(H13), C4(H4),
 C5(H5), C15(H15), N6A(H6A), C14(H14), C20A(H20A), C19A(H19A), C18A(H18A),
 C18B(H18B), N6B(H6B), C19B(H19B), C20B(H20B)
5.b Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C)
;
_shelx_res_checksum              15159
_olex2_submission_special_instructions 'No special instructions were received'