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_7059542
_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, 2(C2 H3 N)'
_chemical_formula_sum            'C27 H28 Mo2 N10 O9'
_chemical_formula_weight         828.47
_chemical_name_systematic
'2,2'-(carbonylbis(hydrazin-2-yl-1-ylidenemethylylidene))di(4-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                75.325(4)
_cell_angle_beta                 74.393(4)
_cell_angle_gamma                85.158(4)
_cell_formula_units_Z            2
_cell_length_a                   8.6152(4)
_cell_length_b                   13.1856(7)
_cell_length_c                   15.5721(8)
_cell_measurement_reflns_used    6967
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      31.6180
_cell_measurement_theta_min      2.3640
_cell_volume                     1647.89(15)
_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 (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 0.999
_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  0.0488
_diffrn_reflns_av_unetI/netI     0.0770
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            18887
_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         29.499
_diffrn_reflns_theta_min         2.362
_exptl_absorpt_coefficient_mu    0.827
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82403
_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 red'
_exptl_crystal_density_diffrn    1.670
_exptl_crystal_description       block
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.800
_refine_diff_density_min         -0.662
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     443
_refine_ls_number_reflns         9170
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0724
_refine_ls_R_factor_gt           0.0443
_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^)+(0.0391P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0906
_refine_ls_wR_factor_ref         0.1001
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6740
_reflns_number_total             9170
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj01045f2.cif
_cod_data_source_block           6b_2CH3CN
_cod_depositor_comments
;Adding full bibliography for 7059536--7059543.cif.

 Adding full bibliography for 7059536--7059543.cif.
;
_cod_database_code               7059542
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.922
_shelx_estimated_absorpt_t_min   0.789
_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
 H6-N6
 0.88 with sigma of 0.02
3. Rigid body (RIGU) restrains
 C26, N10
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Aromatic/amide H refined with riding coordinates:
 C9(H9), C18(H18), C21(H21), C12(H12), C23(H23), C20(H20), C7(H7), C19(H19),
 C22(H22), C15(H15), C3(H3), C6(H6A), C14(H14), C5(H5)
4.b Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C16(H16A,H16B,H16C), C25(H25A,H25B,H25C), C27(H27A,H27B,
 H27C)
;
_shelx_res_checksum              64294
_olex2_submission_special_instructions 'No special instructions were received'