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_7059808
_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         'C20 H18 Mo N6 O4, 2(Mo3 O9.5), 2(C2 H3 N)'
_chemical_formula_sum            'C24 H24 Mo7 N8 O23'
_chemical_formula_weight         1464.09
_chemical_name_systematic
'(mu-N''-(2-oxynaphthylidene)-N'''-(3-pyridinium)carbonohydrazido)(N-acetonitrile)-dioxomolybdenum(vi) hexamolybdate acetonitrile solvate'
_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   geom
_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                 134.52(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   45.012(7)
_cell_length_b                   11.4125(5)
_cell_length_c                   21.787(4)
_cell_measurement_reflns_used    5640
_cell_measurement_temperature    150
_cell_measurement_theta_max      20.6390
_cell_measurement_theta_min      4.1640
_cell_volume                     7980(5)
_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 (Sheldrick, 2015)'
_diffrn_ambient_temperature      150
_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 0.995
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     -4.00 102.00   1.00   15.00    --   28.34  37.00 -90.00  106
  2  \w    -25.00  73.00   1.00   15.00    --   28.34 -99.00 -90.00   98
  3  \w   -102.00  -8.00   1.00   15.00    --  -31.31 -57.00  60.00   94
  4  \w    -98.00  44.00   1.00   15.00    --  -31.31  19.00 -30.00  142
  5  \w   -104.00   2.00   1.00   15.00    --  -31.31 -77.00 -90.00  106
  6  \w   -111.00 -34.00   1.00   15.00    --  -31.31-179.00  60.00   77
  7  \w   -102.00  -8.00   1.00   15.00    --  -31.31 -57.00 -30.00   94
  8  \w     -5.00 101.00   1.00   15.00    --   28.34  77.00 -90.00  106
  9  \w     34.00 108.00   1.00   15.00    --   28.34 179.00 120.00   74
 10  \w     34.00 108.00   1.00   15.00    --   28.34 179.00  90.00   74
 11  \w   -111.00 -34.00   1.00   15.00    --  -31.31-179.00   0.00   77
 12  \w   -104.00   2.00   1.00   15.00    --  -31.31 -77.00  90.00  106
 13  \w   -102.00  -8.00   1.00   15.00    --  -31.31 -57.00 150.00   94
 14  \w   -104.00   2.00   1.00   15.00    --  -31.31 -77.00   0.00  106
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0141932000
_diffrn_orient_matrix_UB_12      -0.0093192000
_diffrn_orient_matrix_UB_13      0.0450641000
_diffrn_orient_matrix_UB_21      -0.0163033000
_diffrn_orient_matrix_UB_22      0.0090724000
_diffrn_orient_matrix_UB_23      -0.0021624000
_diffrn_orient_matrix_UB_31      -0.0046087000
_diffrn_orient_matrix_UB_32      -0.0607359000
_diffrn_orient_matrix_UB_33      -0.0072039000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2144
_diffrn_reflns_av_unetI/netI     0.0948
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       52
_diffrn_reflns_limit_h_min       -52
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            77186
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        24.712
_diffrn_reflns_theta_max         24.712
_diffrn_reflns_theta_min         4.031
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.225
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83666
_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            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.437
_exptl_crystal_description       prism
_exptl_crystal_F_000             5616
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.080
_refine_diff_density_min         -0.975
_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     566
_refine_ls_number_reflns         6786
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.1178
_refine_ls_R_factor_gt           0.0717
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0350P)^2^+48.3992P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1088
_refine_ls_wR_factor_ref         0.1216
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4672
_reflns_number_total             6786
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj03106b2.cif
_cod_data_source_block           '[MoO2(H2L3pynaf)(CH3CN)]Mo6O19x2CH3CN'
_cod_depositor_comments
;Adding full bibliography for 7059802--7059812.cif.

 Adding full bibliography for 7059802--7059812.cif.
;
_cod_original_cell_volume        7980(3)
_cod_database_code               7059808
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C20 Mo7 O25'
_chemical_oxdiff_usercomment     '3pynaf+MoO2acac2 1:7 acn'
_shelx_estimated_absorpt_t_max   0.897
_shelx_estimated_absorpt_t_min   0.665
_reflns_odcompleteness_completeness 99.39
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.66
_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.a Aromatic/amide H refined with riding coordinates:
 N3(H3), N2(H2), C7(H7), C4(H4), C14(H14), C11(H11), C9(H9), C18(H18), N5(H5),
 C3(H3A), C13(H13), C17(H17), C16(H16), C15(H15), C12(H12)
2.b Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C24(H24A,H24B,H24C), C22(H22A,H22B,H22C)
;
_shelx_res_checksum              89617
_olex2_date_sample_data_collection 2019-04-24
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.257
_oxdiff_exptl_absorpt_empirical_full_min 0.872