#------------------------------------------------------------------------------
#$Date: 2019-11-05 12:05:13 +0200 (Tue, 05 Nov 2019) $
#$Revision: 223324 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/16/7701637.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_7701637
loop_
_publ_author_name
'Hay, Moya A.'
'Sarkar, Arup'
'Marriott, Katie E. R.'
'Wilson, Claire'
'Rajaraman, Gopalan'
'Murrie, Mark'
_publ_section_title
;
 Investigation of the magnetic anisotropy in a series of trigonal
 bipyramidal Mn(ii) complexes.
;
_journal_issue                   41
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15480
_journal_page_last               15486
_journal_paper_doi               10.1039/c9dt02187f
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C12 H25 Cl3 Mn1 N4'
_chemical_formula_sum            'C12 H25 Cl3 Mn N4'
_chemical_formula_weight         386.65
_space_group_crystal_system      trigonal
_space_group_IT_number           155
_space_group_name_Hall           'R 3 2"'
_space_group_name_H-M_alt        'R 3 2 :H'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2015-10-29
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2018-11-23 deposited with the CCDC.	2019-06-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   10.628(3)
_cell_length_b                   10.628(3)
_cell_length_c                   12.506(3)
_cell_measurement_reflns_used    1608
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.74
_cell_measurement_theta_min      2.75
_cell_volume                     1223.4(6)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2, (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0702
_diffrn_reflns_av_unetI/netI     0.0379
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            4341
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.743
_diffrn_reflns_theta_min         2.748
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.296
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7301
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1121 before and 0.0898 after correction.
The Ratio of minimum to maximum transmission is 0.7301.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.574
_exptl_crystal_description       needle
_exptl_crystal_F_000             603
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.268
_refine_diff_density_min         -0.283
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.03(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     34
_refine_ls_number_reflns         529
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0225
_refine_ls_R_factor_gt           0.0221
_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/[σ²(Fo²)+(0.0224P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0516
_refine_ls_wR_factor_ref         0.0518
_reflns_Friedel_coverage         0.706
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                522
_reflns_number_total             529
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9dt02187f2.cif
_cod_data_source_block           complex1
_cod_original_sg_symbol_H-M      'R 3 2'
_cod_database_code               7701637
_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.
;
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.97(4) 0.03(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All N(H) groups
3. Others
 Fixed Sof: H2(0.16667)
4.a Secondary CH2 refined with riding coordinates:
 C1(H1B,H1A), C2(H2A,H2B)
;
_shelx_res_file
;
    km562_0m.res created by SHELXL-2014/7

TITL KM562_0m in R32
REM Instructions for potential hydrogen bonds
CELL 0.71075 10.6284 10.6284 12.5057 90 90 120
ZERR 3 0.0025 0.0025 0.0029 0 0 0
LATT -3
SYMM -Y,+X-Y,+Z
SYMM +Y-X,-X,+Z
SYMM -Y+X,-Y,-Z
SYMM -X,-X+Y,-Z
SYMM +Y,+X,-Z
SFAC C H Cl Mn N
UNIT 36 75 9 3 12
EQIV $1 0.667-Y+X,1.333-Y,1.333-Z
EQIV $2 1-Y,1+X-Y,+Z
EQIV $3 -0.333+Y-X,0.333-X,0.333+Z
EQIV $4 0.667+X,0.333+Y,0.333+Z

L.S. 4 0 0
PLAN  20
TEMP -173(2)
HTAB N2 N2_$1
HTAB C1 Cl1_$2
HTAB C1 Cl1_$3
HTAB C2 Cl1_$3
HTAB C2 Cl1_$4
MORE -1
BOND $H
CONF
fmap 2 53
acta
SHEL 100 0.77
TWIN -1 0 0 0 -1 0 0 0 -1 2
REM <olex2.extras>
REM <HklSrc "%.\\KM562_0m.hkl">
REM </olex2.extras>

WGHT    0.022400
BASF   0.02887
FVAR       0.13513
MN1   4    0.333333    0.666667    0.166667    10.16667    0.01111    0.01111 =
         0.00810    0.00000    0.00000    0.00555
CL1   3    0.107065    0.440399    0.166667    10.50000    0.01385    0.01385 =
         0.01391    0.00008   -0.00008    0.00261
N1    5    0.333333    0.666667    0.355649    10.33333    0.01169    0.01169 =
         0.01165    0.00000    0.00000    0.00585
N2    5    0.333333    0.666667    0.560988    10.33333    0.01211    0.01211 =
         0.00810    0.00000    0.00000    0.00606
H2    2    0.333333    0.666667    0.636403    10.16667   -1.50000
C1    1    0.346327    0.542952    0.397703    11.00000    0.02436    0.01576 =
         0.01142    0.00003   -0.00031    0.01398
AFIX  23
H1B   2    0.430647    0.542914    0.364099    11.00000   -1.20000
H1A   2    0.257865    0.450378    0.379276    11.00000   -1.20000
AFIX   0
C2    1    0.366159    0.554772    0.520564    11.00000    0.01684    0.01489 =
         0.01073    0.00143    0.00083    0.00915
AFIX  23
H2A   2    0.299948    0.459810    0.554156    11.00000   -1.20000
H2B   2    0.467241    0.582126    0.539094    11.00000   -1.20000
AFIX   0
HKLF 4

REM  KM562_0m in R32
REM R1 =  0.0221 for     522 Fo > 4sig(Fo)  and  0.0225 for all     529 data
REM     34 parameters refined using      0 restraints

END

WGHT      0.0224      0.0000

REM Highest difference peak  0.268,  deepest hole -0.283,  1-sigma level  0.054
Q1    1   0.4439  0.6667  0.1667  10.50000  0.05    0.27
Q2    1   0.3755  0.7470  0.2138  11.00000  0.05    0.25
Q3    1   0.1792  0.4573  0.2218  11.00000  0.05    0.22
Q4    1   0.3647  0.5338  0.4548  11.00000  0.05    0.20
Q5    1   0.0102  0.4467  0.1948  11.00000  0.05    0.18
Q6    1   0.4067  0.5484  0.5265  11.00000  0.05    0.18
Q7    1   0.2272  0.6667  0.1667  10.50000  0.05    0.17
Q8    1   0.4036  0.7354  0.5701  11.00000  0.05    0.17
Q9    1   0.1374  0.3965  0.2185  11.00000  0.05    0.17
Q10   1   0.1049  0.5533  0.1764  11.00000  0.05    0.16
Q11   1   0.3815  0.7381  0.3792  11.00000  0.05    0.16
Q12   1   0.2425  0.3370  0.5336  11.00000  0.05    0.16
Q13   1   0.0287  0.3814  0.2080  11.00000  0.05    0.15
Q14   1   0.1670  0.4961  0.1103  11.00000  0.05    0.15
Q15   1   0.3741  0.7294  0.3130  11.00000  0.05    0.14
Q16   1   0.4661  0.6327  0.4686  11.00000  0.05    0.14
Q17   1   0.3333  0.6667  0.2812  10.33333  0.05    0.13
Q18   1   0.2590  0.5272  0.3663  11.00000  0.05    0.13
Q19   1   0.3160  0.4670  0.3689  11.00000  0.05    0.13
Q20   1   0.4086  0.6383  0.5433  11.00000  0.05    0.13
;
_shelx_res_checksum              5538
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, -y, -z'
'-x, -x+y, -z'
'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-y+2/3, -y+1/3, -z+1/3'
'-x+2/3, -x+y+1/3, -z+1/3'
'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+1/3, -y+2/3, -z+2/3'
'-x+1/3, -x+y+2/3, -z+2/3'
'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
Mn1 Mn 0.3333 0.6667 0.1667 0.0101(3) Uani 1 6 d S T P
Cl1 Cl 0.10707(9) 0.44040(9) 0.1667 0.0158(3) Uani 1 2 d S T P
N1 N 0.3333 0.6667 0.3556(3) 0.0117(8) Uani 1 3 d S T P
N2 N 0.3333 0.6667 0.5610(3) 0.0108(8) Uani 1 3 d S T P
H2 H 0.3333 0.6667 0.636(7) 0.016 Uiso 0.5 3 d RS T P
C1 C 0.3463(3) 0.5430(3) 0.3977(2) 0.0154(7) Uani 1 1 d . . .
H1B H 0.4306 0.5429 0.3641 0.019 Uiso 1 1 calc R . .
H1A H 0.2579 0.4504 0.3793 0.019 Uiso 1 1 calc R . .
C2 C 0.3662(3) 0.5548(3) 0.5206(2) 0.0136(6) Uani 1 1 d . . .
H2A H 0.2999 0.4598 0.5542 0.016 Uiso 1 1 calc R . .
H2B H 0.4672 0.5821 0.5391 0.016 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Mn1 0.0111(4) 0.0111(4) 0.0081(5) 0.000 0.000 0.00555(19)
Cl1 0.0138(4) 0.0138(4) 0.0139(5) 0.00008(19) -0.00008(19) 0.0026(4)
N1 0.0117(12) 0.0117(12) 0.0117(18) 0.000 0.000 0.0058(6)
N2 0.0121(12) 0.0121(12) 0.0081(18) 0.000 0.000 0.0061(6)
C1 0.0244(15) 0.0158(14) 0.0114(14) 0.0000(11) -0.0003(11) 0.0140(11)
C2 0.0168(15) 0.0149(13) 0.0107(12) 0.0014(10) 0.0008(11) 0.0091(12)
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'
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
Cl1 Mn1 Cl1 120.0 3_565 2_665
Cl1 Mn1 Cl1 120.0 3_565 .
Cl1 Mn1 Cl1 120.0 . 2_665
N1 Mn1 Cl1 90.000(1) 10_565 .
N1 Mn1 Cl1 90.0 . 2_665
N1 Mn1 Cl1 90.0 . .
N1 Mn1 Cl1 90.0 . 3_565
N1 Mn1 Cl1 90.0 10_565 3_565
N1 Mn1 Cl1 90.000(1) 10_565 2_665
N1 Mn1 N1 180.0 . 10_565
C1 N1 Mn1 110.73(16) 3_565 .
C1 N1 Mn1 110.74(16) 2_665 .
C1 N1 Mn1 110.74(16) . .
C1 N1 C1 108.18(17) 3_565 2_665
C1 N1 C1 108.18(17) 3_565 .
C1 N1 C1 108.18(17) 2_665 .
C2 N2 H2 109.90(17) 3_565 .
C2 N2 H2 109.90(16) . .
C2 N2 H2 109.90(16) 2_665 .
C2 N2 C2 109.04(16) 2_665 .
C2 N2 C2 109.04(16) 3_565 .
C2 N2 C2 109.04(16) 3_565 2_665
N1 C1 H1B 109.6 . .
N1 C1 H1A 109.6 . .
N1 C1 C2 110.4(2) . .
H1B C1 H1A 108.1 . .
C2 C1 H1B 109.6 . .
C2 C1 H1A 109.6 . .
N2 C2 C1 109.0(2) . .
N2 C2 H2A 109.9 . .
N2 C2 H2B 109.9 . .
C1 C2 H2A 109.9 . .
C1 C2 H2B 109.9 . .
H2A C2 H2B 108.3 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn1 Cl1 2.4048(11) 3_565
Mn1 Cl1 2.4049(11) 2_665
Mn1 Cl1 2.4049(11) .
Mn1 N1 2.363(3) .
Mn1 N1 2.363(3) 10_565
N1 C1 1.485(3) 2_665
N1 C1 1.485(3) .
N1 C1 1.485(3) 3_565
N2 H2 0.94(8) .
N2 C2 1.485(3) 2_665
N2 C2 1.485(3) .
N2 C2 1.485(3) 3_565
C1 H1B 0.9900 .
C1 H1A 0.9900 .
C1 C2 1.547(4) .
C2 H2A 0.9900 .
C2 H2B 0.9900 .
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
N2 H2 N2 0.94(8) 1.70(8) 2.643(7) 180.000(1) 10_566
C1 H1B Cl1 0.99 2.81 3.498(3) 127.0 2_665
C1 H1A Cl1 0.99 2.99 3.758(3) 135.3 9_455
C2 H2A Cl1 0.99 2.98 3.717(3) 132.2 9_455
C2 H2B Cl1 0.99 2.89 3.764(3) 147.4 7
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
Mn1 N1 C1 C2 172.73(16) .
N1 C1 C2 N2 12.5(3) .
C1 N1 C1 C2 -65.8(2) 3_565
C1 N1 C1 C2 51.2(3) 2_665
C2 N2 C2 C1 -66.7(2) 2_665
C2 N2 C2 C1 52.3(3) 3_565
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.97(4)
2 0.03(4)
