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_7059810
_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         'C28 H22 Mo2 N10 O8, 2(C2 H3 N)'
_chemical_formula_sum            'C32 H28 Mo2 N12 O8'
_chemical_formula_weight         900.54
_chemical_name_systematic
'bis((mu-N''-(2-oxybenzylidene)-N'''-(3-pyridyl)carbonohydrazido))-tetraoxo-di-molybdenum(vi) acetonitrile solvate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-01-07
_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                 116.102(9)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.3525(9)
_cell_length_b                   13.6312(8)
_cell_length_c                   12.5586(8)
_cell_measurement_reflns_used    2696
_cell_measurement_temperature    298
_cell_measurement_theta_max      24.3880
_cell_measurement_theta_min      3.1220
_cell_volume                     1745.2(2)
_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      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 0.895
_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    -38.00  11.00   1.00   39.00    --   22.34 -37.00-180.00   49
  2  \w    -25.00  40.00   1.00   39.00    --   22.34 -37.00   0.00   65
  3  \w     55.00  88.00   1.00   39.00    --   22.34  57.00  30.00   33
  4  \w      8.00  67.00   1.00   39.00    --   22.34  57.00 -90.00   59
  5  \w    -47.00  92.00   1.00   39.00    --   22.34   0.00-150.00  139
  6  \w     63.00  90.00   1.00   39.00    --   22.34 179.00-120.00   27
  7  \w     60.00  87.00   1.00   39.00    --   22.34 179.00 -30.00   27
  8  \w     -4.00  45.00   1.00   39.00    --   22.34  19.00   0.00   49
;
_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      0.0502359000
_diffrn_orient_matrix_UB_12      0.0354296000
_diffrn_orient_matrix_UB_13      0.0271060000
_diffrn_orient_matrix_UB_21      -0.0257607000
_diffrn_orient_matrix_UB_22      0.0117069000
_diffrn_orient_matrix_UB_23      0.0406728000
_diffrn_orient_matrix_UB_31      0.0406492000
_diffrn_orient_matrix_UB_32      -0.0362864000
_diffrn_orient_matrix_UB_33      0.0395274000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1097
_diffrn_reflns_av_unetI/netI     0.2347
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.895
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            21021
_diffrn_reflns_point_group_measured_fraction_full 0.957
_diffrn_reflns_point_group_measured_fraction_max 0.810
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.944
_diffrn_reflns_theta_min         3.230
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.789
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97511
_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    1.714
_exptl_crystal_description       plate
_exptl_crystal_F_000             904
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.065
_refine_diff_density_min         -1.202
_refine_diff_density_rms         0.152
_refine_ls_abs_structure_details
;
 Flack x determined using 1405 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.01(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.954
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     489
_refine_ls_number_reflns         10637
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.954
_refine_ls_R_factor_all          0.1846
_refine_ls_R_factor_gt           0.0793
_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^)+(0.0117P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0857
_refine_ls_wR_factor_ref         0.1123
_reflns_Friedel_coverage         0.748
_reflns_Friedel_fraction_full    0.914
_reflns_Friedel_fraction_max     0.720
_reflns_number_gt                5239
_reflns_number_total             10637
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj03106b2.cif
_cod_data_source_block           '[MoO2(L3pysal)]2x2CH3CN'
_cod_depositor_comments
;Adding full bibliography for 7059802--7059812.cif.

 Adding full bibliography for 7059802--7059812.cif.
;
_cod_database_code               7059810
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Mo2 O8 C26 N10'
_shelx_estimated_absorpt_t_max   0.962
_shelx_estimated_absorpt_t_min   0.925
_reflns_odcompleteness_completeness 99.31
_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
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N3(H3), N3A(H3A), C12(H12), C7(H7), C9(H9), C13(H13), C6A(H6A), C13A(H13A),
 C12A(H12A), C7A(H7A), C11A(H11A), C9A(H9A), C14(H14), C3(H3B), C11(H11),
 C5A(H5A), C6(H6), C4A(H4A), C14A(H14A), C4(H4), C5(H5), C3A(H3AA)
2.b Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C16A(H16D,H16E,H16F)
;
_shelx_res_checksum              42758
_olex2_date_sample_data_collection 2017-03-09
_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 1.072
_oxdiff_exptl_absorpt_empirical_full_min 0.957