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_7059804
_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(C14 H14 N5 O2)'
_chemical_formula_sum            'C28 H28 Mo6 N10 O23'
_chemical_formula_weight         1448.24
_chemical_name_systematic
'bis[2-(4-pyridinium)-2'-(2-hydroxyphenyl)-(carbonylbis(hydrazin-2-yl-1-ylidenemethylylidene)] hexamolybdate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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                 106.419(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.1525(5)
_cell_length_b                   17.7564(7)
_cell_length_c                   13.2831(9)
_cell_measurement_reflns_used    4995
_cell_measurement_temperature    298
_cell_measurement_theta_max      32.3360
_cell_measurement_theta_min      4.5660
_cell_volume                     2070.7(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
;
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 0.870
_diffrn_measurement_details
;
  1 omega   -4.00   22.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       22.3432   19.0000    0.0000 26

  2 omega   -1.00   91.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       22.3432   19.0000   90.0000 92

  3 omega   64.00   90.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       22.3432   19.0000    0.0000 26

  4 omega  -16.00   46.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       22.3432  -99.0000  -60.0000 62

  5 omega  -84.00  -58.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.4994 -179.0000  -30.0000 26

  6 omega   46.00   91.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       22.3432  179.0000  -60.0000 45
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0619733000
_diffrn_orient_matrix_UB_12      0.0118680000
_diffrn_orient_matrix_UB_13      0.0424608000
_diffrn_orient_matrix_UB_21      0.0064089000
_diffrn_orient_matrix_UB_22      0.0333760000
_diffrn_orient_matrix_UB_23      -0.0277289000
_diffrn_orient_matrix_UB_31      -0.0513765000
_diffrn_orient_matrix_UB_32      0.0184336000
_diffrn_orient_matrix_UB_33      0.0230516000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0345
_diffrn_reflns_av_unetI/netI     0.0556
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.870
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            15212
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.870
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.967
_diffrn_reflns_theta_min         4.085
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.862
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75391
_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    2.323
_exptl_crystal_description       prism
_exptl_crystal_F_000             1404
_exptl_crystal_preparation
'Slow hydrolysis of acetonitrile solution of L4pysal and MoO2(acac)2.'
_exptl_crystal_recrystallization_method 'Same as preparation.'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.923
_refine_diff_density_min         -0.726
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         6769
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0629
_refine_ls_R_factor_gt           0.0393
_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^)+(0.0276P)^2^+0.6332P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0737
_refine_ls_wR_factor_ref         0.0839
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5095
_reflns_number_total             6769
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj03106b2.cif
_cod_data_source_block           (H3L4pysal)2Mo6O19
_cod_depositor_comments
;Adding full bibliography for 7059802--7059812.cif.

 Adding full bibliography for 7059802--7059812.cif.
;
_cod_database_code               7059804
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         Mo
_chemical_oxdiff_usercomment     Mo(acac)2+4pysal-acn
_shelx_estimated_absorpt_t_max   0.913
_shelx_estimated_absorpt_t_min   0.707
_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
 N5-H5
 0.84 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C9(H9), C7(H7), C11(H11), C14(H14), C13(H13), C6(H6), C12(H12), C3(H3A),
 C5(H5A), C4(H4)
;
_shelx_res_checksum              62456
_olex2_exptl_crystal_mounting_method 'Glass fiber/shellac'
_olex2_submission_special_instructions 'No special instructions were received'