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_7059537
_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         'C19 H22 Mo2 N4 O11, 0.64(C O)'
_chemical_formula_sum            'C19.64 H22 Mo2 N4 O11.64'
_chemical_formula_weight         692.21
_chemical_name_systematic
'2,2'-(carbonylbis(hydrazin-2-yl-1-ylidenemethylylidene))di(3-methoxyphenolato))bis(methanol)tetraoxo-di-molybdenum(vi)methanol 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             2019-07-19
_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                112.516(5)
_cell_angle_beta                 98.637(4)
_cell_angle_gamma                97.085(5)
_cell_formula_units_Z            2
_cell_length_a                   7.4466(4)
_cell_length_b                   13.8570(9)
_cell_length_c                   14.0640(8)
_cell_measurement_reflns_used    4165
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.1060
_cell_measurement_theta_min      2.8320
_cell_volume                     1299.16(15)
_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(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.3426
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0916
_diffrn_reflns_av_unetI/netI     0.1160
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            22707
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.500
_diffrn_reflns_theta_min         2.710
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.031
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79835
_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            orange
_exptl_crystal_density_diffrn    1.774
_exptl_crystal_description       prism
_exptl_crystal_F_000             689.9
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.262
_refine_diff_density_min         -1.167
_refine_diff_density_rms         0.193
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     356
_refine_ls_number_reflns         7244
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.1156
_refine_ls_R_factor_gt           0.0633
_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^)+(0.0511P)^2^+0.9217P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1267
_refine_ls_wR_factor_ref         0.1477
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4564
_reflns_number_total             7246
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj01045f2.cif
_cod_data_source_block           5a_064_CH3OH
_cod_depositor_comments
;Adding full bibliography for 7059536--7059543.cif.

 Adding full bibliography for 7059536--7059543.cif.
;
_cod_original_cell_volume        1299.16(14)
_cod_database_code               7059537
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H) groups, All C(H,H,H) groups
2. Restrained distances
 Mo2-O7B
 1.7 with sigma of 0.005
 Mo2-O7A
 1.7 with sigma of 0.005
 Mo2-O6B
 1.7 with sigma of 0.005
 Mo2-O6A
 1.7 with sigma of 0.005
 Mo2-O11B
 2.3 with sigma of 0.01
 O11A-C19A
 1.4 with sigma of 0.02
 O11B-C19B
 1.4 with sigma of 0.02
 O10-H10
 0.84 with sigma of 0.01
 O11A-H11A
 0.84 with sigma of 0.01
 O11B-H11B
 0.84 with sigma of 0.01
 O12A-C20A
 1.4 with sigma of 0.02
 O12B-C20B
 1.4 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(Mo2) = Uanis(O11B) = Uanis(C19B)
Uanis(Mo2) = Uanis(O7B)
Uanis(Mo2) = Uanis(O7A)
Uanis(Mo2) = Uanis(O6B)
Uanis(Mo2) = Uanis(O6A)
4. Others
 Sof(O6B)=Sof(O11B)=Sof(C19B)=Sof(H19D)=Sof(H19E)=Sof(H19F)=Sof(O7B)=Sof(H11B)=
 1-FVAR(1)
 Sof(O7A)=Sof(O11A)=Sof(O6A)=Sof(C19A)=Sof(H19A)=Sof(H19B)=Sof(H19C)=Sof(H11A)=
 FVAR(1)
 Fixed Sof: O12A(0.32) C20B(0.32) O12B(0.32) C20A(0.32)
5.a Aromatic/amide H refined with riding coordinates:
 C15(H15), C14(H14), C13(H13), C7(H7), C9(H9), C6(H6), C4(H4), C5(H5)
5.b Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C16(H16A,H16B,H16C), C19A(H19A,H19B,
 H19C), C19B(H19D,H19E,H19F)
;
_shelx_res_checksum              34562
_olex2_submission_special_instructions 'No special instructions were received'