#------------------------------------------------------------------------------
#$Date: 2016-01-09 12:29:36 +0200 (Sat, 09 Jan 2016) $
#$Revision: 173753 $
#$URL: svn://www.crystallography.net/cod/cif/7/22/30/7223098.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_7223098
loop_
_publ_author_name
'Hu, Tuoping'
'Zheng, Baohua'
'Wang, Xiaoqing'
'Hao, Xuena'
_publ_section_title
;
 Syntheses, structures and magnetic properties of four manganese(ii) and
 cobalt(ii) complexes
;
_journal_issue                   48
_journal_name_full               CrystEngComm
_journal_page_first              9348
_journal_paper_doi               10.1039/C5CE01857A
_journal_volume                  17
_journal_year                    2015
_chemical_formula_moiety         'C23 H18 Mn N2 O6, H2 O'
_chemical_formula_sum            'C23 H20 Mn N2 O7'
_chemical_formula_weight         491.35
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-01-25
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.19 svn.r3143 for OlexSys, GUI svn.r4992)
;
_audit_update_record
;
2015-01-25 deposited with the CCDC.
2015-10-29 downloaded from the CCDC.
;
_cell_angle_alpha                96.781(7)
_cell_angle_beta                 94.868(7)
_cell_angle_gamma                110.509(7)
_cell_formula_units_Z            2
_cell_length_a                   7.7565(6)
_cell_length_b                   9.5643(8)
_cell_length_c                   15.1895(14)
_cell_measurement_reflns_used    1852
_cell_measurement_temperature    298.5(4)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2.93
_cell_volume                     1038.34(16)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      298.5(4)
_diffrn_detector_area_resol_mean 16.0450
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
  1 omega   16.00   48.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8251  -86.0000  -34.0556 32

  2 omega  -48.00   21.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8251  -57.0000 -150.0000 69

  3 omega  -30.00   85.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8251   19.0000   30.0000 115

  4 omega   50.00   97.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8251  178.0000 -120.0000 47

  5 omega   -2.00   84.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8251   57.0000   90.0000 86

  6 omega   -2.00   24.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8251   57.0000  -30.0000 26

  7 omega  -20.00   24.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.9813  -99.0000 -180.0000 44

  8 omega  -77.00  -51.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.9813  -19.0000   60.0000 26

  9 omega  -55.00  -30.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8251  -19.0000  -60.0000 25
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0359309000
_diffrn_orient_matrix_UB_12      0.0521064000
_diffrn_orient_matrix_UB_13      0.0403422000
_diffrn_orient_matrix_UB_21      0.0482202000
_diffrn_orient_matrix_UB_22      0.0567779000
_diffrn_orient_matrix_UB_23      -0.0245570000
_diffrn_orient_matrix_UB_31      -0.0780717000
_diffrn_orient_matrix_UB_32      0.0221803000
_diffrn_orient_matrix_UB_33      -0.0047318000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0630
_diffrn_reflns_av_unetI/netI     0.1019
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            8071
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.93
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.686
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84969
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            faint-yellow
_exptl_crystal_density_diffrn    1.572
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             506
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.458
_refine_diff_density_min         -0.348
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         3631
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0887
_refine_ls_R_factor_gt           0.0536
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0166P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0810
_refine_ls_wR_factor_ref         0.0983
_reflns_number_gt                2495
_reflns_number_total             3631
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ce01857a2.cif
_cod_data_source_block           htp-f14
_cod_depositor_comments
'Adding full bibliography for 7223097--7223100.cif.'
_cod_original_cell_volume        1038.33(15)
_cod_database_code               7223098
_audit_block_doi                 10.5517/cc141rtr
_chemical_oxdiff_formula         'C H O N Co'
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2.a Free rotating group:
 O3W(H3WA,H3WB)
2.b Rotating group:
 O2W(H2WB), O1W(H1WB,H1WA)
2.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C17(H17), C18(H18), C10(H10), C20(H20), C4(H4), C0AA(H0AA), C13(H13),
 C5(H5), C2(H2), C11(H11), C14(H14), C8(H8), C9(H9)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, -y, -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_calc_flag
_atom_site_refinement_flags_posn
Mn1 Mn 0.70621(7) 0.12265(6) 0.41627(4) 0.02803(18) Uani 1 d .
O4 O 0.6056(3) 0.2725(3) 0.35104(17) 0.0317(7) Uani 1 d .
O2 O 0.3190(4) 0.7607(3) 0.46082(18) 0.0389(7) Uani 1 d .
O1 O 0.4514(3) 0.9302(3) 0.37469(19) 0.0404(7) Uani 1 d .
N4 N 0.8893(4) -0.0789(3) 0.1837(2) 0.0289(8) Uani 1 d .
O3 O 0.3275(4) 0.2325(3) 0.3980(2) 0.0444(8) Uani 1 d .
O3W O 0.9195(4) 0.5589(3) 0.3720(3) 0.0697(11) Uani 1 d .
H3WA H 0.8199 0.4816 0.3590 0.105 Uiso 1 d G
H3WB H 1.0040 0.5349 0.3981 0.105 Uiso 1 d G
O2W O 1.0096(4) 0.2973(4) 0.4463(3) 0.0498(9) Uani 1 d .
H2WB H 1.0839 0.2606 0.4196 0.075 Uiso 1 d GR
N8 N 0.8223(4) 0.0562(3) 0.2961(2) 0.0340(8) Uani 1 d .
C3 C 0.9835(4) -0.4375(4) 0.0279(3) 0.0274(9) Uani 1 d .
O1W O 0.8069(4) -0.0232(3) 0.4974(2) 0.0724(12) Uani 1 d .
H1WB H 0.8765 -0.0589 0.4683 0.109 Uiso 1 d GR
H1WA H 0.7131 -0.0970 0.5075 0.109 Uiso 1 d GR
C15 C 0.4654(5) 0.3034(4) 0.1540(2) 0.0239(9) Uani 1 d .
C16 C 0.4550(4) 0.4315(4) 0.2183(2) 0.0232(9) Uani 1 d .
C7 C 0.8567(5) -0.0670(4) 0.2697(3) 0.0324(10) Uani 1 d .
H7 H 0.8583 -0.1379 0.3064 0.039 Uiso 1 calc R
C21 C 0.4360(4) 0.4235(4) 0.3086(2) 0.0216(8) Uani 1 d .
C12 C 0.4899(5) 0.0620(4) 0.0314(2) 0.0232(9) Uani 1 d .
C6 C 0.9203(5) -0.2004(4) 0.1315(3) 0.0279(9) Uani 1 d .
C17 C 0.4576(4) 0.5632(4) 0.1867(3) 0.0270(9) Uani 1 d .
H17 H 0.4698 0.5708 0.1269 0.032 Uiso 1 calc R
C18 C 0.4426(4) 0.6832(4) 0.2422(2) 0.0260(9) Uani 1 d .
H18 H 0.4495 0.7711 0.2198 0.031 Uiso 1 calc R
C19 C 0.4174(4) 0.6730(4) 0.3311(2) 0.0249(9) Uani 1 d .
C10 C 0.3719(5) 0.1511(4) 0.1620(2) 0.0267(9) Uani 1 d .
H10 H 0.2998 0.1275 0.2079 0.032 Uiso 1 calc R
C20 C 0.4131(4) 0.5407(4) 0.3627(2) 0.0245(9) Uani 1 d .
H20 H 0.3943 0.5311 0.4217 0.029 Uiso 1 calc R
C22 C 0.4552(5) 0.2969(4) 0.3563(3) 0.0275(9) Uani 1 d .
C4 C 0.9172(5) -0.3375(4) -0.0113(3) 0.0322(10) Uani 1 d .
H4 H 0.8946 -0.3491 -0.0733 0.039 Uiso 1 calc R
C23 C 0.3944(5) 0.7987(4) 0.3930(3) 0.0281(9) Uani 1 d .
C0AA C 1.0139(5) -0.4143(4) 0.1209(3) 0.0340(10) Uani 1 d .
H0AA H 1.0546 -0.4803 0.1494 0.041 Uiso 1 calc R
C13 C 0.5791(5) 0.2143(4) 0.0226(3) 0.0303(9) Uani 1 d .
H13 H 0.6484 0.2377 -0.0243 0.036 Uiso 1 calc R
C5 C 0.8843(5) -0.2220(4) 0.0395(3) 0.0325(10) Uani 1 d .
H5 H 0.8377 -0.1587 0.0115 0.039 Uiso 1 calc R
C2 C 0.9858(5) -0.2966(4) 0.1730(3) 0.0334(10) Uani 1 d .
H2 H 1.0107 -0.2828 0.2351 0.040 Uiso 1 calc R
C11 C 0.3861(5) 0.0361(4) 0.1022(3) 0.0278(9) Uani 1 d .
H11 H 0.3233 -0.0633 0.1097 0.033 Uiso 1 calc R
C14 C 0.5663(5) 0.3305(4) 0.0823(3) 0.0318(10) Uani 1 d .
H14 H 0.6271 0.4298 0.0742 0.038 Uiso 1 calc R
C8 C 0.8763(5) 0.0485(4) 0.1533(3) 0.0393(11) Uani 1 d .
H8 H 0.8921 0.0737 0.0965 0.047 Uiso 1 calc R
C9 C 0.8359(5) 0.1294(5) 0.2226(3) 0.0389(11) Uani 1 d .
H9 H 0.8198 0.2210 0.2209 0.047 Uiso 1 calc R
H2WA H 1.048(8) 0.316(7) 0.495(4) 0.12(3) Uiso 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'
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
O4 Mn1 O1 93.66(9) . 1_545
O4 Mn1 O2W 93.12(11) . .
O4 Mn1 N8 92.87(10) . .
O4 Mn1 O1W 174.36(12) . .
O2 Mn1 O4 87.16(9) 2_666 .
O2 Mn1 O1 107.93(11) 2_666 1_545
O2 Mn1 O2W 82.36(13) 2_666 .
O2 Mn1 N8 161.82(11) 2_666 .
O2 Mn1 O1W 87.22(11) 2_666 .
O1 Mn1 O2W 167.94(11) 1_545 .
O1 Mn1 N8 90.22(11) 1_545 .
O1 Mn1 O1W 87.70(10) 1_545 .
N8 Mn1 O2W 79.49(13) . .
N8 Mn1 O1W 92.59(12) . .
O1W Mn1 O2W 86.52(12) . .
C22 O4 Mn1 129.3(2) . .
C23 O2 Mn1 135.2(3) . 2_666
C23 O1 Mn1 133.1(2) . 1_565
C7 N4 C6 128.2(3) . .
C7 N4 C8 105.7(3) . .
C8 N4 C6 126.1(3) . .
C7 N8 Mn1 131.2(3) . .
C7 N8 C9 104.8(3) . .
C9 N8 Mn1 122.7(2) . .
C4 C3 C3 121.2(4) . 2_745
C0AA C3 C3 122.6(4) . 2_745
C0AA C3 C4 116.2(3) . .
C10 C15 C16 122.1(3) . .
C14 C15 C16 121.2(3) . .
C14 C15 C10 116.7(3) . .
C21 C16 C15 123.2(3) . .
C17 C16 C15 119.1(3) . .
C17 C16 C21 117.7(3) . .
N8 C7 N4 112.8(3) . .
C16 C21 C22 124.1(3) . .
C20 C21 C16 120.4(3) . .
C20 C21 C22 115.3(3) . .
C13 C12 C12 121.1(4) . 2_655
C11 C12 C12 123.1(4) . 2_655
C11 C12 C13 115.8(3) . .
C5 C6 N4 119.9(3) . .
C5 C6 C2 119.8(4) . .
C2 C6 N4 120.3(3) . .
C18 C17 C16 121.7(3) . .
C17 C18 C19 120.5(3) . .
C18 C19 C20 117.9(3) . .
C18 C19 C23 122.3(3) . .
C20 C19 C23 119.8(3) . .
C11 C10 C15 120.6(4) . .
C21 C20 C19 121.7(3) . .
O4 C22 C21 115.7(3) . .
O3 C22 O4 127.0(3) . .
O3 C22 C21 117.3(3) . .
C5 C4 C3 122.0(4) . .
O2 C23 C19 115.5(3) . .
O1 C23 O2 125.2(4) . .
O1 C23 C19 119.3(4) . .
C2 C0AA C3 122.6(3) . .
C14 C13 C12 121.5(4) . .
C6 C5 C4 120.1(3) . .
C6 C2 C0AA 119.2(4) . .
C10 C11 C12 123.2(3) . .
C13 C14 C15 122.2(4) . .
C9 C8 N4 106.7(4) . .
C8 C9 N8 110.1(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn1 O4 2.152(2) .
Mn1 O2 2.119(3) 2_666
Mn1 O1 2.158(3) 1_545
Mn1 O2W 2.328(3) .
Mn1 N8 2.226(3) .
Mn1 O1W 2.254(2) .
O4 C22 1.274(4) .
O2 Mn1 2.119(3) 2_666
O2 C23 1.256(4) .
O1 Mn1 2.158(3) 1_565
O1 C23 1.252(4) .
N4 C7 1.351(5) .
N4 C6 1.430(4) .
N4 C8 1.385(4) .
O3 C22 1.238(4) .
N8 C7 1.322(4) .
N8 C9 1.378(5) .
C3 C3 1.492(7) 2_745
C3 C4 1.401(4) .
C3 C0AA 1.391(5) .
C15 C16 1.504(5) .
C15 C10 1.407(4) .
C15 C14 1.390(5) .
C16 C21 1.400(5) .
C16 C17 1.395(4) .
C21 C20 1.381(4) .
C21 C22 1.526(4) .
C12 C12 1.493(6) 2_655
C12 C13 1.404(4) .
C12 C11 1.392(5) .
C6 C5 1.379(5) .
C6 C2 1.383(4) .
C17 C18 1.386(5) .
C18 C19 1.391(5) .
C19 C20 1.396(4) .
C19 C23 1.508(5) .
C10 C11 1.382(5) .
C4 C5 1.382(5) .
C0AA C2 1.390(5) .
C13 C14 1.386(5) .
C8 C9 1.356(5) .
