#------------------------------------------------------------------------------
#$Date: 2019-11-07 21:34:14 +0200 (Thu, 07 Nov 2019) $
#$Revision: 223546 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/21/7232129.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_7232129
loop_
_publ_author_name
'Chalmers, James E.'
'Srivastava, Anant Kumar'
'Dixey, Richard J. C.'
'Sivakumaran, Krrishna'
'Saines, Paul J.'
_publ_section_title
;
 Low dimensional and frustrated antiferromagnetic interactions in
 transition metal chloride complexes with simple amine ligands
;
_journal_issue                   5
_journal_name_full               CrystEngComm
_journal_page_first              894
_journal_paper_doi               10.1039/C8CE01901K
_journal_volume                  21
_journal_year                    2019
_chemical_formula_moiety         'Cl2 Co H14 N4 O2, 2(Cl)'
_chemical_formula_sum            'Cl4 Co H14 N4 O2'
_chemical_formula_weight         302.88
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2018-02-05
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3461 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-11-06 deposited with the CCDC.
2018-12-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.745(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.9880(6)
_cell_length_b                   5.7019(5)
_cell_length_c                   11.3808(8)
_cell_measurement_reflns_used    1105
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.9940
_cell_measurement_theta_min      4.0100
_cell_volume                     513.63(7)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2887
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.867
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -20.00  28.00   1.00   11.83    --  -10.46 -99.00 -30.00   48
  2  ω    -39.00  13.00   1.00   11.83    --  -10.46 -38.00   0.00   52
  3  ω    -36.00  52.00   1.00   11.83    --   11.79 -19.00 150.00   88
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0891536000
_diffrn_orient_matrix_UB_12      0.0077140000
_diffrn_orient_matrix_UB_13      0.0034795000
_diffrn_orient_matrix_UB_21      0.0072269000
_diffrn_orient_matrix_UB_22      -0.1195771000
_diffrn_orient_matrix_UB_23      0.0171891000
_diffrn_orient_matrix_UB_31      -0.0053242000
_diffrn_orient_matrix_UB_32      -0.0335763000
_diffrn_orient_matrix_UB_33      -0.0603818000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0311
_diffrn_reflns_av_unetI/netI     0.0513
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.867
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            2489
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.867
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.487
_diffrn_reflns_theta_min         3.613
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.677
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93868
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.958
_exptl_crystal_description       blade
_exptl_crystal_F_000             306
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.439
_refine_diff_density_min         -0.429
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     54
_refine_ls_number_reflns         1236
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0311
_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)+(0.0169P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0548
_refine_ls_wR_factor_ref         0.0602
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1053
_reflns_number_total             1236
_reflns_threshold_expression     'I > 2σ(I)'
_iucr_refine_instructions_details
;

    18_pjs040.res created by SHELXL-2014/7

TITL 18_pjs040_a.res in P2(1)/c
REM Old TITL 18_PJS040 in P21/c #14
REM SHELXT solution in P2(1)/c
REM R1 0.086, Rweak 0.003, Alpha 0.017, Orientation as input
REM Formula found by SHELXT: N6 Mn Cl4
CELL 0.71073 7.987998 5.70189 11.380785 90 97.7453 90
ZERR 2 0.000643 0.000489 0.000798 0 0.0069 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC Cl Co H N O
UNIT 8 2 28 8 4
 
L.S. 10
PLAN  20
BOND $H
LIST 6
MORE -1
CONF
fmap 2
acta 52
REM <olex2.extras>
REM <HklSrc "%./18_PJS040.hkl">
REM </olex2.extras>
 
WGHT    0.016900
FVAR       0.77577
CO1   2    0.500000    0.500000    0.500000    10.50000    0.01529    0.01485 =
         0.01436    0.00040    0.00061   -0.00102
CL1   1    0.491962    0.809178    0.355531    11.00000    0.02542    0.01939 =
         0.01790    0.00283    0.00460    0.00130
CL2   1    0.962513    0.685340    0.358745    11.00000    0.02345    0.02919 =
         0.02346    0.00094    0.00281    0.00056
O1    5    0.312786    0.684544    0.582064    11.00000    0.02262    0.02354 =
         0.02091   -0.00583    0.00242   -0.00348
AFIX   7
H1A   3    0.356186    0.742454    0.650304    11.00000   -1.50000
H1B   3    0.236776    0.587184    0.600964    11.00000   -1.50000
AFIX   0
N1    4    0.706690    0.655393    0.617261    11.00000    0.01989    0.02009 =
         0.01817   -0.00004    0.00141   -0.00071
AFIX  23
H1C   3    0.665778    0.695609    0.683390    11.00000   -1.20000
H1D   3    0.781861    0.542038    0.636901    11.00000   -1.20000
AFIX   0
N2    4    0.799223    0.855487    0.582206    11.00000    0.02096    0.02206 =
         0.02800   -0.00341    0.00412   -0.00358
AFIX 137
H2A   3    0.850726    0.817189    0.520262    11.00000   -1.20000
H2B   3    0.875937    0.899088    0.642301    11.00000   -1.20000
H2C   3    0.728018    0.973465    0.562457    11.00000   -1.20000
AFIX   0
HKLF 4
 
REM  18_pjs040_a.res in P2(1)/c
REM R1 =  0.0311 for    1053 Fo > 4sig(Fo)  and  0.0429 for all    1236 data
REM     54 parameters refined using      0 restraints
 
END  
     
WGHT      0.0169      0.0000 

REM Highest difference peak  0.439,  deepest hole -0.429,  1-sigma level  0.118
Q1    1   0.3574  0.7945  0.2781  11.00000  0.05    0.44
Q2    1   1.0766  0.6660  0.4555  11.00000  0.05    0.44
Q3    1   0.3716  0.8848  0.3657  11.00000  0.05    0.41
Q4    1   1.0111  0.6981  0.3191  11.00000  0.05    0.41
Q5    1   0.2538  0.4882  0.5358  11.00000  0.05    0.39
Q6    1   0.7292  1.1561  0.6532  11.00000  0.05    0.38
Q7    1   1.0000  0.5000  0.5000  10.50000  0.05    0.37
Q8    1   1.1026  0.7062  0.2620  11.00000  0.05    0.37
Q9    1   0.0137  0.6074  0.5804  11.00000  0.05    0.37
Q10   1   0.9565  1.0012  0.7239  11.00000  0.05    0.36
Q11   1   0.8890  0.6146  0.6045  11.00000  0.05    0.36
Q12   1   0.8649  0.4960  0.2869  11.00000  0.05    0.34
Q13   1   0.3972  0.6420  0.4659  11.00000  0.05    0.34
Q14   1   0.5868  0.9973  0.3373  11.00000  0.05    0.33
Q15   1   0.6684  0.7840  0.7401  11.00000  0.05    0.33
Q16   1   0.9350  0.6847  0.4527  11.00000  0.05    0.33
Q17   1   0.8376  0.8562  0.4170  11.00000  0.05    0.32
Q18   1   0.5040  0.9657  0.4598  11.00000  0.05    0.32
Q19   1   0.3062  1.0090  0.6765  11.00000  0.05    0.32
Q20   1   1.0625  0.6065  0.4040  11.00000  0.05    0.32

  REM The information below was added by Olex2.
  REM
  REM R1 = 0.0311 for 1053 Fo > 4sig(Fo) and 0.0429 for all 2678 data
  REM n/a parameters refined using n/a restraints
  REM Highest difference peak 0.44, deepest hole -0.43
  REM Mean Shift 0, Max Shift 0.000.

  REM +++ Tabular Listing of Refinement Information +++
  REM R1_all = 0.0429
  REM R1_gt = 0.0311
  REM wR_ref = 0.0602
  REM GOOF = 1.050
  REM Shift_max = 0.000
  REM Shift_mean = 0
  REM Reflections_all = 2678
  REM Reflections_gt = 1053
  REM Parameters = n/a
  REM Hole = -0.43
  REM Peak = 0.44
  REM Flack = n/a

  
;
_cod_data_source_file            c8ce01901k2.cif
_cod_data_source_block           18_pjs040_Hyd2CoCl4
_cod_depositor_comments
'Adding full bibliography for 7232129--7232133.cif.'
_cod_database_code               7232129
_shelx_shelxl_version_number     2014/7
_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.
;
_reflns_odcompleteness_completeness 99.65
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Rotating group:
 O1(H1A,H1B)
2.b Secondary CH2 refined with riding coordinates:
 N1(H1C,H1D)
2.c Idealised Me refined as rotating group:
 N2(H2A,H2B,H2C)
;
_olex2_date_sample_data_collection 2018-01-18
_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 1.062
_oxdiff_exptl_absorpt_empirical_full_min 0.938
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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
Co1 Co 0.5000 0.5000 0.5000 0.01496(14) Uani 1 2 d S T P
Cl1 Cl 0.49196(8) 0.80918(12) 0.35553(5) 0.02075(16) Uani 1 1 d . . .
Cl2 Cl 0.96251(8) 0.68534(13) 0.35875(5) 0.02540(18) Uani 1 1 d . . .
O1 O 0.3128(2) 0.6845(3) 0.58206(14) 0.0224(4) Uani 1 1 d . . .
H1A H 0.3562 0.7425 0.6503 0.034 Uiso 1 1 d GR . .
H1B H 0.2368 0.5872 0.6010 0.034 Uiso 1 1 d GR . .
N1 N 0.7067(3) 0.6554(4) 0.61726(15) 0.0195(5) Uani 1 1 d . . .
H1C H 0.6658 0.6956 0.6834 0.023 Uiso 1 1 calc R . .
H1D H 0.7819 0.5420 0.6369 0.023 Uiso 1 1 calc R . .
N2 N 0.7992(3) 0.8555(4) 0.58221(17) 0.0236(5) Uani 1 1 d . . .
H2A H 0.8507 0.8172 0.5203 0.028 Uiso 1 1 calc GR . .
H2B H 0.8759 0.8991 0.6423 0.028 Uiso 1 1 calc GR . .
H2C H 0.7280 0.9735 0.5625 0.028 Uiso 1 1 calc GR . .
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
Co1 0.0153(3) 0.0148(3) 0.0144(2) 0.00040(19) 0.00061(17) -0.0010(2)
Cl1 0.0254(4) 0.0194(4) 0.0179(3) 0.0028(2) 0.0046(2) 0.0013(3)
Cl2 0.0235(4) 0.0292(4) 0.0235(3) 0.0009(3) 0.0028(2) 0.0006(3)
O1 0.0226(10) 0.0235(11) 0.0209(8) -0.0058(8) 0.0024(7) -0.0035(8)
N1 0.0199(11) 0.0201(13) 0.0182(9) 0.0000(9) 0.0014(8) -0.0007(10)
N2 0.0210(12) 0.0221(14) 0.0280(11) -0.0034(10) 0.0041(9) -0.0036(10)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 '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'
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 Co1 Cl1 180.00(3) . 3_666
O1 Co1 Cl1 91.02(5) . 3_666
O1 Co1 Cl1 88.98(5) . .
O1 Co1 Cl1 91.02(5) 3_666 .
O1 Co1 Cl1 88.98(5) 3_666 3_666
O1 Co1 O1 180.0 . 3_666
O1 Co1 N1 92.83(7) 3_666 3_666
O1 Co1 N1 87.17(7) 3_666 .
O1 Co1 N1 92.83(7) . .
O1 Co1 N1 87.17(7) . 3_666
N1 Co1 Cl1 86.03(6) . 3_666
N1 Co1 Cl1 93.97(6) . .
N1 Co1 Cl1 86.03(6) 3_666 .
N1 Co1 Cl1 93.97(6) 3_666 3_666
N1 Co1 N1 180.0 . 3_666
Co1 O1 H1A 110.9 . .
Co1 O1 H1B 110.2 . .
H1A O1 H1B 103.2 . .
Co1 N1 H1C 106.9 . .
Co1 N1 H1D 106.9 . .
H1C N1 H1D 106.7 . .
N2 N1 Co1 121.90(13) . .
N2 N1 H1C 106.9 . .
N2 N1 H1D 106.9 . .
N1 N2 H2A 109.5 . .
N1 N2 H2B 109.5 . .
N1 N2 H2C 109.5 . .
H2A N2 H2B 109.5 . .
H2A N2 H2C 109.5 . .
H2B N2 H2C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 Cl1 2.4056(6) 3_666
Co1 Cl1 2.4056(6) .
Co1 O1 2.1430(18) .
Co1 O1 2.1430(18) 3_666
Co1 N1 2.1675(19) 3_666
Co1 N1 2.1675(19) .
O1 H1A 0.8717 .
O1 H1B 0.8708 .
N1 H1C 0.8900 .
N1 H1D 0.8900 .
N1 N2 1.445(3) .
N2 H2A 0.8900 .
N2 H2B 0.8900 .
N2 H2C 0.8900 .
