#------------------------------------------------------------------------------
#$Date: 2021-07-05 20:05:48 +0200 (lun 05 de jul de 2021) $
#$Revision: 267220 $
#$URL: svn://www.crystallography.net/cod/cif/7/06/06/7060625.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7060625
loop_
_publ_author_name
'Braun, Vanessa'
'Wurzenberger, Maximilian H. H.'
'Weippert, Valentin'
'Stierstorfer, Jörg'
_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 H36 Mn N24, 2(Cl O4)'
_chemical_formula_sum            'C24 H36 Cl2 Mn N24 O8'
_chemical_formula_weight         914.61
_chemical_name_common
'hexakis(1-cyclopropyl-5H-tetrazolyl)manganese(II) diperchlorate'
_chemical_name_systematic
'hexakis(1-cyclopropyl-5H-tetrazolyl)manganese(II) diperchlorate'
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      148
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     difmap
_audit_creation_date             2020-06-05
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   10.8880(6)
_cell_length_b                   10.8880(6)
_cell_length_c                   29.5174(17)
_cell_measurement_reflns_used    1240
_cell_measurement_temperature    106(2)
_cell_measurement_theta_max      30.1090
_cell_measurement_theta_min      2.5280
_cell_volume                     3030.4(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.81a (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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -70.00  -3.00   1.00   30.00    --  -24.42 -57.00-180.00   67
  2  ω    -24.00  39.00   1.00   30.00    --   25.20 -57.00 -90.00   63
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0409365000
_diffrn_orient_matrix_UB_12      0.0084596000
_diffrn_orient_matrix_UB_13      0.0196922000
_diffrn_orient_matrix_UB_21      0.0631017000
_diffrn_orient_matrix_UB_22      0.0412100000
_diffrn_orient_matrix_UB_23      -0.0125853000
_diffrn_orient_matrix_UB_31      -0.0019232000
_diffrn_orient_matrix_UB_32      0.0622747000
_diffrn_orient_matrix_UB_33      0.0056583000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0146
_diffrn_reflns_av_sigmaI/netI    0.0276
_diffrn_reflns_av_unetI/netI     0.0261
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            2261
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.328
_diffrn_reflns_theta_min         2.070
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.535
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93090
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.81a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.503
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1413
_exptl_crystal_size_max          0.642
_exptl_crystal_size_mid          0.594
_exptl_crystal_size_min          0.142
_refine_diff_density_max         0.329
_refine_diff_density_min         -0.323
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     114
_refine_ls_number_reflns         1385
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0352
_refine_ls_R_factor_gt           0.0293
_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/[σ²(Fo²)+(0.0367P)²+2.7176P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0734
_refine_ls_wR_factor_ref         0.0768
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1240
_reflns_number_total             1385
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1nj01675j2.cif
_cod_data_source_block           px217
_cod_depositor_comments
'Adding full bibliography for 7060620--7060640.cif.'
_cod_original_cell_volume        3030.4(4)
_cod_original_sg_symbol_H-M      'R -3 '
_cod_database_code               7060625
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.725
_shelx_estimated_absorpt_t_max   0.928
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.666667 0.333333 0.333333 0.01444(16) Uani 1 6 d S T P . .
Cl1 Cl 0.333333 0.666667 0.32421(2) 0.01978(18) Uani 1 3 d S T P . .
N4 N 0.38038(13) 0.41233(13) 0.41608(4) 0.0176(3) Uani 1 1 d . . . . .
O1 O 0.42915(14) 0.62244(14) 0.34103(5) 0.0345(3) Uani 1 1 d . . . . .
N1 N 0.53711(14) 0.39488(13) 0.37699(4) 0.0186(3) Uani 1 1 d . . . . .
N3 N 0.50839(14) 0.51123(15) 0.43185(5) 0.0234(3) Uani 1 1 d . . . . .
O2 O 0.333333 0.666667 0.27611(7) 0.0456(7) Uani 1 3 d S T P . .
N2 N 0.60225(14) 0.50008(14) 0.40845(5) 0.0235(3) Uani 1 1 d . . . . .
C1 C 0.40019(16) 0.34322(16) 0.38253(5) 0.0189(3) Uani 1 1 d . . . . .
C2 C 0.25087(16) 0.40580(18) 0.43134(5) 0.0202(3) Uani 1 1 d . . . . .
C3 C 0.22800(19) 0.40598(19) 0.48121(6) 0.0253(4) Uani 1 1 d . . . . .
C4 C 0.14224(19) 0.2737(2) 0.45415(6) 0.0276(4) Uani 1 1 d . . . . .
H2 H 0.2199(18) 0.4518(19) 0.4116(6) 0.019(4) Uiso 1 1 d . . . . .
H3A H 0.298(2) 0.409(2) 0.5007(7) 0.028(5) Uiso 1 1 d . . . . .
H1 H 0.327(2) 0.270(2) 0.3678(6) 0.022(4) Uiso 1 1 d . . . . .
H4A H 0.046(2) 0.2448(19) 0.4471(7) 0.028(5) Uiso 1 1 d . . . . .
H3B H 0.187(2) 0.460(2) 0.4900(6) 0.027(5) Uiso 1 1 d . . . . .
H4B H 0.163(2) 0.200(2) 0.4574(7) 0.034(5) Uiso 1 1 d . . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Mn1 N1 90.36(5) . 3_665 ?
N1 Mn1 N1 90.36(5) . 2_655 ?
N1 Mn1 N1 90.36(5) 3_665 2_655 ?
N1 Mn1 N1 89.65(5) . 17 ?
N1 Mn1 N1 89.64(5) 3_665 17 ?
N1 Mn1 N1 180.0 2_655 17 ?
N1 Mn1 N1 89.64(5) . 18_545 ?
N1 Mn1 N1 180.0 3_665 18_545 ?
N1 Mn1 N1 89.64(5) 2_655 18_545 ?
N1 Mn1 N1 90.36(5) 17 18_545 ?
N1 Mn1 N1 180.0 . 16_655 ?
N1 Mn1 N1 89.64(5) 3_665 16_655 ?
N1 Mn1 N1 89.64(5) 2_655 16_655 ?
N1 Mn1 N1 90.35(5) 17 16_655 ?
N1 Mn1 N1 90.35(5) 18_545 16_655 ?
O2 Cl1 O1 110.18(6) . 3_565 ?
O2 Cl1 O1 110.18(6) . . ?
O1 Cl1 O1 108.75(6) 3_565 . ?
O2 Cl1 O1 110.18(6) . 2_665 ?
O1 Cl1 O1 108.75(6) 3_565 2_665 ?
O1 Cl1 O1 108.75(6) . 2_665 ?
C1 N4 N3 108.34(13) . . ?
C1 N4 C2 129.48(14) . . ?
N3 N4 C2 121.62(13) . . ?
C1 N1 N2 106.06(13) . . ?
C1 N1 Mn1 133.70(11) . . ?
N2 N1 Mn1 120.01(9) . . ?
N2 N3 N4 106.95(12) . . ?
N3 N2 N1 109.86(12) . . ?
N1 C1 N4 108.77(14) . . ?
N1 C1 H1 128.9(12) . . ?
N4 C1 H1 122.3(12) . . ?
N4 C2 C4 118.13(14) . . ?
N4 C2 C3 117.76(14) . . ?
C4 C2 C3 60.22(12) . . ?
N4 C2 H2 112.5(11) . . ?
C4 C2 H2 118.3(11) . . ?
C3 C2 H2 120.6(11) . . ?
C2 C3 C4 59.79(11) . . ?
C2 C3 H3A 117.8(12) . . ?
C4 C3 H3A 117.3(12) . . ?
C2 C3 H3B 114.0(12) . . ?
C4 C3 H3B 119.3(12) . . ?
H3A C3 H3B 116.4(17) . . ?
C2 C4 C3 59.98(11) . . ?
C2 C4 H4A 115.4(11) . . ?
C3 C4 H4A 119.1(11) . . ?
C2 C4 H4B 117.1(13) . . ?
C3 C4 H4B 117.8(13) . . ?
H4A C4 H4B 115.7(17) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mn1 N1 2.2461(13) . ?
Mn1 N1 2.2461(13) 3_665 ?
Mn1 N1 2.2461(13) 2_655 ?
Mn1 N1 2.2461(13) 17 ?
Mn1 N1 2.2461(13) 18_545 ?
Mn1 N1 2.2462(13) 16_655 ?
Cl1 O2 1.420(2) . ?
Cl1 O1 1.4383(12) 3_565 ?
Cl1 O1 1.4383(12) . ?
Cl1 O1 1.4384(12) 2_665 ?
N4 C1 1.325(2) . ?
N4 N3 1.3483(19) . ?
N4 C2 1.4478(19) . ?
N1 C1 1.314(2) . ?
N1 N2 1.3655(19) . ?
N3 N2 1.2884(19) . ?
C1 H1 0.906(19) . ?
C2 C4 1.490(2) . ?
C2 C3 1.493(2) . ?
C2 H2 0.935(18) . ?
C3 C4 1.497(3) . ?
C3 H3A 0.95(2) . ?
C3 H3B 0.94(2) . ?
C4 H4A 0.96(2) . ?
C4 H4B 0.95(2) . ?
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
? ? ? ? ? ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
? ? ? ? ? ? ? ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 N4 N3 N2 -0.63(17) . . . . ?
C2 N4 N3 N2 -172.84(14) . . . . ?
N4 N3 N2 N1 0.44(17) . . . . ?
C1 N1 N2 N3 -0.08(18) . . . . ?
Mn1 N1 N2 N3 -175.34(10) . . . . ?
N2 N1 C1 N4 -0.32(17) . . . . ?
Mn1 N1 C1 N4 174.00(10) . . . . ?
N3 N4 C1 N1 0.59(17) . . . . ?
C2 N4 C1 N1 171.99(14) . . . . ?
C1 N4 C2 C4 69.9(2) . . . . ?
N3 N4 C2 C4 -119.73(17) . . . . ?
C1 N4 C2 C3 139.07(17) . . . . ?
N3 N4 C2 C3 -50.5(2) . . . . ?
N4 C2 C3 C4 -108.22(17) . . . . ?
N4 C2 C4 C3 107.61(17) . . . . ?
