Coordinating and supramolecular prospects of unsymmetrically substituted carbohydrazides
Topić, Edi; Landripet, Ivana; Duguin, Maëlle; Pisk, Jana; Đilović, Ivica; Vrdoljak, Višnja; Rubčić, Mirta; New Journal of Chemistry 44 (2020) 13357–13367; doi:10.1039/D0NJ03106B

data_7059812
_publ_section_title
;
 Coordinating and supramolecular prospects of unsymmetrically substituted
 carbohydrazides
;
_journal_issue                   31
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              13357
_journal_page_last               13367
_journal_paper_doi               10.1039/D0NJ03106B
_journal_volume                  44
_journal_year                    2020
_chemical_formula_moiety         'Mo6 O19, 2(C18 H16 N5 O2)'
_chemical_formula_sum            'C36 H32 Mo6 N10 O23'
_chemical_formula_weight         1548.35
_chemical_name_systematic
'bis[2-(4-pyridinium)-2'-(2-hydroxynaphthyl)-(carbonylbis(hydrazin-2-yl-1-ylidenemethylylidene)] hexamolybdate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-12-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-02-27 deposited with the CCDC.	2020-07-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.236(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.3887(3)
_cell_length_b                   17.2816(5)
_cell_length_c                   14.7114(6)
_cell_measurement_reflns_used    8825
_cell_measurement_temperature    298
_cell_measurement_theta_max      29.9290
_cell_measurement_theta_min      4.4320
_cell_volume                     2303.05(14)
_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
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      298
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.3426
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.912
_diffrn_measurement_details
;
  1 omega   -3.00   89.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -       22.3432   77.0000   30.0000 92

  2 omega   -3.00   89.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -       22.3432   77.0000  150.0000 92

  3 omega  -12.00   68.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -       22.3432 -114.0000  -25.0000 80

  4 omega  -43.00   37.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -       22.3432  -57.0000    0.0000 80

  5 omega  -25.00   59.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -       22.3432  -99.0000   90.0000 84

  6 omega  -47.00   92.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -       22.3432    0.0000   60.0000 139

  7 omega    7.00   88.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -       22.3432   57.0000  -90.0000 81

  8 omega  -93.00  -41.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -      -22.4994  179.0000  120.0000 52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0189615000
_diffrn_orient_matrix_UB_12      -0.0381567000
_diffrn_orient_matrix_UB_13      -0.0166015000
_diffrn_orient_matrix_UB_21      0.0147704000
_diffrn_orient_matrix_UB_22      -0.0134137000
_diffrn_orient_matrix_UB_23      0.0471287000
_diffrn_orient_matrix_UB_31      -0.0744989000
_diffrn_orient_matrix_UB_32      0.0070501000
_diffrn_orient_matrix_UB_33      -0.0002244000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0854
_diffrn_reflns_av_unetI/netI     0.0772
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.912
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            43795
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.912
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.970
_diffrn_reflns_theta_min         4.192
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.683
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85983
_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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.233
_exptl_crystal_description       prism
_exptl_crystal_F_000             1508
_exptl_crystal_preparation
'Slow hydrolysis of acetonitrile solution of L4pynaf and MoO2(acac)2.'
_exptl_crystal_recrystallization_method 'Same as preparation'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.842
_refine_diff_density_min         -0.949
_refine_diff_density_rms         0.178
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         7902
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0920
_refine_ls_R_factor_gt           0.0476
_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^)+(0.0355P)^2^+0.6409P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0852
_refine_ls_wR_factor_ref         0.1005
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5336
_reflns_number_total             7902
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj03106b2.cif
_cod_data_source_block           (H3L4pynaf)2Mo6O19
_cod_depositor_comments
;Adding full bibliography for 7059802--7059812.cif.

 Adding full bibliography for 7059802--7059812.cif.
;
_cod_database_code               7059812
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         Mo
_chemical_oxdiff_usercomment     4pynaf+MoO2(acac)2-acn-presuseno
_shelx_estimated_absorpt_t_max   0.921
_shelx_estimated_absorpt_t_min   0.850
_reflns_odcompleteness_completeness 99.68
_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 C(H,H,H,H,H) groups
2. Restrained distances
 O1-H1
 0.82 with sigma of 0.02
 N2-H2 = N3-H3 = N5-H5
 0.88 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C9(H9), C3(H3A), C4(H4), C11(H11), C18(H18), C12(H12), C13(H13),
 C17(H17), C15(H15), C16(H16), C14(H14)
;
_shelx_res_checksum              53905
_olex2_exptl_crystal_mounting_method 'Glass fiber/shellac'
_olex2_submission_special_instructions 'No special instructions were received'