#------------------------------------------------------------------------------
#$Date: 2019-11-05 12:05:13 +0200 (Tue, 05 Nov 2019) $
#$Revision: 223324 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/16/7701639.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_7701639
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         'C7 H17 Cl3 Mn N2 O'
_chemical_formula_sum            'C7 H17 Cl3 Mn N2 O'
_chemical_formula_weight         306.51
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2015-11-16
_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                 96.572(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.8885(19)
_cell_length_b                   9.447(3)
_cell_length_c                   8.269(2)
_cell_measurement_reflns_used    1590
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.55
_cell_measurement_theta_min      2.60
_cell_volume                     612.2(3)
_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 0.998
_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  0.1121
_diffrn_reflns_av_unetI/netI     0.0602
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            11656
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.683
_diffrn_reflns_theta_min         2.479
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.704
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8193
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1178 before and 0.0980 after correction.
The Ratio of minimum to maximum transmission is 0.8193.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.663
_exptl_crystal_description       needle
_exptl_crystal_F_000             314
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.860
_refine_diff_density_min         -0.487
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     85
_refine_ls_number_reflns         1236
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.131
_refine_ls_R_factor_all          0.0636
_refine_ls_R_factor_gt           0.0445
_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)+(0.0380P)²+0.8815P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0981
_refine_ls_wR_factor_ref         0.1059
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1004
_reflns_number_total             1236
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9dt02187f2.cif
_cod_data_source_block           complex3
_cod_database_code               7701639
_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. Fixed Uiso
 At 1.2 times of:
  {H1a,H1b} of C1, {H2a,H2b} of C2, {H4a,H4b} of C4, {H3a,H3b} of C3
 At 1.5 times of:
  {H5a,H5b} of C5
2. Restrained distances
 C5-H5b = C5-H5a
 0.98 with sigma of 0.02
 C5-H5a = C5-H5b
 0.96 with sigma of 0.02
3. Others
 Fixed Sof: H1a(0.5) H1b(0.5) H2a(0.5) H2b(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C1(H1a,H1b), C2(H2a,H2b), C3(H3a,H3b), C4(H4a,H4b)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, z'
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 0.56349(11) 0.7500 0.23819(10) 0.0139(3) Uani 1 2 d S T P
Cl1 Cl 0.69847(13) 0.52687(11) 0.18349(12) 0.0185(3) Uani 1 1 d . . .
Cl2 Cl 0.28915(16) 0.7500 0.33495(16) 0.0113(3) Uani 1 2 d S T P
O1 O 0.4670(5) 0.7500 -0.0224(5) 0.0202(10) Uani 1 2 d S T P
H1 H 0.422(6) 0.828(5) -0.068(6) 0.051(17) Uiso 1 1 d . . .
N1 N 0.7193(6) 0.7500 0.4969(6) 0.0132(10) Uani 1 2 d S T P
N2 N 0.8975(6) 0.7500 0.7782(5) 0.0142(10) Uani 1 2 d S T P
C1 C 0.9026(7) 0.7500 0.4806(7) 0.0177(13) Uani 1 2 d S T P
H1A H 0.9301 0.8347 0.4181 0.021 Uiso 0.5 1 calc R . .
H1B H 0.9301 0.6653 0.4181 0.021 Uiso 0.5 1 calc R . .
C2 C 1.0134(7) 0.7500 0.6442(7) 0.0170(13) Uani 1 2 d S T P
H2A H 1.0873 0.6650 0.6535 0.020 Uiso 0.5 1 calc R . .
H2B H 1.0873 0.8350 0.6535 0.020 Uiso 0.5 1 calc R . .
C3 C 0.6816(5) 0.6232(5) 0.5921(5) 0.0213(10) Uani 1 1 d . . .
H3A H 0.7061 0.5371 0.5306 0.026 Uiso 1 1 calc R . .
H3B H 0.5588 0.6224 0.6066 0.026 Uiso 1 1 calc R . .
C4 C 0.7867(5) 0.6197(4) 0.7586(5) 0.0182(9) Uani 1 1 d . . .
H4A H 0.7098 0.6170 0.8452 0.022 Uiso 1 1 calc R . .
H4B H 0.8589 0.5338 0.7684 0.022 Uiso 1 1 calc R . .
C5 C 1.0001(8) 0.7500 0.9415(7) 0.0175(13) Uani 1 2 d DS T P
H5A H 0.926(6) 0.7500 1.026(5) 0.026 Uiso 1 2 d DRS T P
H5B H 1.070(4) 0.835(3) 0.944(5) 0.026 Uiso 1 1 d DR . .
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
Cl1 Mn1 Cl1 120.55(6) 4_575 .
Cl2 Mn1 Cl1 119.70(3) . .
Cl2 Mn1 Cl1 119.70(3) . 4_575
O1 Mn1 Cl1 85.84(6) . 4_575
O1 Mn1 Cl1 85.84(6) . .
O1 Mn1 Cl2 95.90(12) . .
O1 Mn1 N1 168.65(16) . .
N1 Mn1 Cl1 88.55(6) . 4_575
N1 Mn1 Cl1 88.55(6) . .
N1 Mn1 Cl2 95.44(12) . .
Mn1 O1 H1 119(3) . .
C1 N1 Mn1 109.6(3) . .
C1 N1 C3 108.0(3) . 4_575
C1 N1 C3 108.0(3) . .
C3 N1 Mn1 111.6(2) . .
C3 N1 Mn1 111.6(2) 4_575 .
C3 N1 C3 107.9(4) . 4_575
C4 N2 C2 108.2(3) . .
C4 N2 C2 108.2(3) 4_575 .
C4 N2 C4 109.4(4) 4_575 .
C5 N2 C2 110.6(4) . .
C5 N2 C4 110.2(3) . 4_575
C5 N2 C4 110.2(3) . .
N1 C1 H1A 109.0 . .
N1 C1 H1B 109.0 . .
N1 C1 C2 112.9(4) . .
H1A C1 H1B 107.8 . .
C2 C1 H1A 109.0 . .
C2 C1 H1B 109.0 . .
N2 C2 C1 108.4(4) . .
N2 C2 H2A 110.0 . .
N2 C2 H2B 110.0 . .
C1 C2 H2A 110.0 . .
C1 C2 H2B 110.0 . .
H2A C2 H2B 108.4 . .
N1 C3 H3A 109.2 . .
N1 C3 H3B 109.2 . .
N1 C3 C4 112.1(3) . .
H3A C3 H3B 107.9 . .
C4 C3 H3A 109.2 . .
C4 C3 H3B 109.2 . .
N2 C4 C3 109.2(3) . .
N2 C4 H4A 109.8 . .
N2 C4 H4B 109.8 . .
C3 C4 H4A 109.8 . .
C3 C4 H4B 109.8 . .
H4A C4 H4B 108.3 . .
N2 C5 H5A 110(4) . .
N2 C5 H5B 106(3) . .
H5A C5 H5B 112(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn1 Cl1 2.4273(12) 4_575
Mn1 Cl1 2.4273(12) .
Mn1 Cl2 2.3917(16) .
Mn1 O1 2.202(4) .
Mn1 N1 2.342(5) .
O1 H1 0.88(5) .
N1 C1 1.467(7) .
N1 C3 1.482(5) 4_575
N1 C3 1.482(5) .
N2 C2 1.515(7) .
N2 C4 1.508(5) 4_575
N2 C4 1.508(5) .
N2 C5 1.493(7) .
C1 H1A 0.9900 .
C1 H1B 0.9900 .
C1 C2 1.524(8) .
C2 H2A 0.9900 .
C2 H2B 0.9900 .
C3 H3A 0.9900 .
C3 H3B 0.9900 .
C3 C4 1.524(6) .
C4 H4A 0.9900 .
C4 H4B 0.9900 .
C5 H5A 0.964(14) .
C5 H5B 0.976(14) .
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 180.000(1) .
Mn1 N1 C3 C4 178.2(3) .
N1 C1 C2 N2 0.000(1) .
N1 C3 C4 N2 0.9(5) .
C1 N1 C3 C4 57.6(5) .
C2 N2 C4 C3 -59.7(4) .
C3 N1 C1 C2 58.2(3) 4_575
C3 N1 C1 C2 -58.2(3) .
C3 N1 C3 C4 -58.8(5) 4_575
C4 N2 C2 C1 59.2(3) .
C4 N2 C2 C1 -59.2(3) 4_575
C4 N2 C4 C3 58.0(5) 4_575
C5 N2 C2 C1 180.000(1) .
C5 N2 C4 C3 179.3(4) .
