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_7059541
_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         'C17 H18 N4 O5'
_chemical_formula_sum            'C17 H18 N4 O5'
_chemical_formula_weight         358.35
_chemical_name_systematic
1,3-bis[(E)-[(2-hydroxy-4-methoxyphenyl)methylidene]amino]urea
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-07-16
_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                90
_cell_angle_beta                 104.692(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.3305(8)
_cell_length_b                   10.2881(7)
_cell_length_c                   18.0461(16)
_cell_measurement_reflns_used    922
_cell_measurement_temperature    298
_cell_measurement_theta_max      25.7390
_cell_measurement_theta_min      4.5700
_cell_volume                     1675.7(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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    'ShelXD (Sheldrick, 2008)'
_diffrn_ambient_temperature      298
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.3426
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
  1 omega    5.00   88.00   1.0000   37.5000
omega____ theta____ kappa____ phi______ frames
    -       22.3432   37.0000   30.0000 83

  2 omega  -38.00   10.00   1.0000   37.5000
omega____ theta____ kappa____ phi______ frames
    -       22.3432  -57.0000 -150.0000 48

  3 omega   33.00   92.00   1.0000   37.5000
omega____ theta____ kappa____ phi______ frames
    -       22.3432 -179.0000 -120.0000 59

  4 omega    7.00   43.00   1.0000   37.5000
omega____ theta____ kappa____ phi______ frames
    -       22.3432   57.0000   90.0000 36

  5 omega    7.00   87.00   1.0000   37.5000
omega____ theta____ kappa____ phi______ frames
    -       22.3432   57.0000  -90.0000 80

  6 omega   35.00   89.00   1.0000   37.5000
omega____ theta____ kappa____ phi______ frames
    -       22.3432  179.0000    0.0000 54

  7 omega  -10.00   92.00   1.0000   37.5000
omega____ theta____ kappa____ phi______ frames
    -       22.3432    0.0000  -30.0000 102
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0627765000
_diffrn_orient_matrix_UB_12      -0.0352947000
_diffrn_orient_matrix_UB_13      -0.0206153000
_diffrn_orient_matrix_UB_21      0.0471391000
_diffrn_orient_matrix_UB_22      -0.0493886000
_diffrn_orient_matrix_UB_23      -0.0078486000
_diffrn_orient_matrix_UB_31      -0.0033814000
_diffrn_orient_matrix_UB_32      -0.0326777000
_diffrn_orient_matrix_UB_33      0.0341320000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0566
_diffrn_reflns_av_unetI/netI     0.0697
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            7739
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.987
_diffrn_reflns_theta_min         4.130
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.107
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97036
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.420
_exptl_crystal_description       plate
_exptl_crystal_F_000             752
_exptl_crystal_preparation
'Reaction between carbohydrazide and 4-methoxysalicylaldehide in methanol.'
_exptl_crystal_recrystallization_method 'crystallized from methanol'
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.142
_refine_diff_density_min         -0.145
_refine_diff_density_rms         0.037
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     125
_refine_ls_number_reflns         1821
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.1372
_refine_ls_R_factor_gt           0.0664
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0317P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1061
_refine_ls_wR_factor_ref         0.1242
_reflns_Friedel_coverage         0.000
_reflns_number_gt                995
_reflns_number_total             1821
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj01045f2.cif
_cod_data_source_block           H4L6
_cod_depositor_comments
;Adding full bibliography for 7059536--7059543.cif.

 Adding full bibliography for 7059536--7059543.cif.
;
_cod_database_code               7059541
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.995
_shelx_estimated_absorpt_t_min   0.979
_reflns_odcompleteness_completeness 99.70
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N2-H2
 0.86 with sigma of 0.02
 O1-H1
 0.82 with sigma of 0.02
3. Rigid body (RIGU) restrains
 C1, C7
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Me refined with riding coordinates:
 C9(H9A,H9B,H9C)
4.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C7(H7), C6(H6), C3(H3)
;
_shelx_res_checksum              36027
_olex2_exptl_crystal_mounting_method 'mounted on glass fiber with shellac glue'
_olex2_submission_special_instructions 'No special instructions were received'
_publcif_funding_html
;
;