Tailoring the properties of 3d transition metal complexes with different N-cycloalkyl-substituted tetrazoles
Braun, Vanessa; Wurzenberger, Maximilian H. H.; Weippert, Valentin; Stierstorfer, Jörg; New Journal of Chemistry 45 (2021) 11042–11050; doi:10.1039/D1NJ01675J

data_7060637
_publ_section_title
;
 Tailoring the properties of 3d transition metal complexes with different
 N-cycloalkyl-substituted tetrazoles
;
_journal_issue                   25
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              11042
_journal_page_last               11050
_journal_paper_doi               10.1039/D1NJ01675J
_journal_volume                  45
_journal_year                    2021
_chemical_formula_moiety         'C24 H44 Mn N16 O2, 2(Cl O4)'
_chemical_formula_sum            'C24 H44 Cl2 Mn N16 O10'
_chemical_formula_weight         842.59
_chemical_name_common
'diaqua tetrakis(1-cyclopentyl-5H-tetrazole) iron(II) diperchlorate'
_chemical_name_systematic
'diaqua tetrakis(1-cyclopentyl-5H-tetrazole) iron(II) diperchlorate'
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     difmap
_audit_creation_date             2020-09-23
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-02-04 deposited with the CCDC.	2021-04-28 downloaded from the CCDC.
;
_cell_angle_alpha                68.044(4)
_cell_angle_beta                 79.661(4)
_cell_angle_gamma                77.005(4)
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_cell_length_b                   11.9386(6)
_cell_length_c                   15.5566(7)
_cell_measurement_reflns_used    3778
_cell_measurement_temperature    106(2)
_cell_measurement_theta_max      28.8860
_cell_measurement_theta_min      2.2870
_cell_volume                     1788.58(15)
_computing_cell_refinement       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Diamond 2.1c, Crystal Impact GbR'
_computing_publication_material  'Encifer 1.5.1, CCDC 2014'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    SIR-92
_diffrn_ambient_temperature      106(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9809
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.885
_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    -39.00  11.00   1.00   10.00    --  -15.28 -77.00  30.00   50
  2  \w     -3.00  85.00   1.00   10.00    --   16.22  37.00   0.00   88
  3  \w    -20.00  55.00   1.00   10.00    --   16.22 -99.00-180.00   75
  4  \w    -54.00  39.00   1.00   10.00    --   16.22 -19.00-180.00   93
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0603530000
_diffrn_orient_matrix_UB_12      0.0134712000
_diffrn_orient_matrix_UB_13      -0.0176131000
_diffrn_orient_matrix_UB_21      -0.0253737000
_diffrn_orient_matrix_UB_22      -0.0398680000
_diffrn_orient_matrix_UB_23      0.0430237000
_diffrn_orient_matrix_UB_31      -0.0194962000
_diffrn_orient_matrix_UB_32      0.0495884000
_diffrn_orient_matrix_UB_33      0.0168143000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0234
_diffrn_reflns_av_sigmaI/netI    0.0451
_diffrn_reflns_av_unetI/netI     0.0498
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.885
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12525
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.885
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.282
_diffrn_reflns_theta_min         1.961
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.595
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89247
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.82a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.565
_exptl_crystal_description       block
_exptl_crystal_F_000             878
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.300
_refine_diff_density_max         1.724
_refine_diff_density_min         -0.918
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     497
_refine_ls_number_reflns         7870
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0768
_refine_ls_R_factor_gt           0.0572
_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^)+(0.0604P)^2^+3.5768P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1349
_refine_ls_wR_factor_ref         0.1514
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6124
_reflns_number_total             7870
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj01675j2.cif
_cod_data_source_block           px326
_cod_depositor_comments
'Adding full bibliography for 7060620--7060640.cif.'
_cod_database_code               7060637
_shelx_estimated_absorpt_t_min   0.797
_shelx_estimated_absorpt_t_max   0.842
_shelx_res_checksum              59622