#------------------------------------------------------------------------------
#$Date: 2019-11-17 12:10:56 +0200 (Sun, 17 Nov 2019) $
#$Revision: 229799 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/52/7045236.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_7045236
loop_
_publ_author_name
'Chen, Shuai'
'Narayanam, Nagaraju'
'Zhang, Lei'
'Zhang, Jian'
_publ_section_title
;
 Hydrogen bond-assisted homochiral lattice packing between inorganic
 helices built from heterometallic units.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2134
_journal_page_last               2137
_journal_paper_doi               10.1039/c7dt04112h
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         '0.2(C18 H21 Mn6 O42 Ti3)'
_chemical_formula_sum            'C3.6 H4.2 Mn1.2 O8.4 Ti0.6'
_chemical_formula_weight         276.54
_space_group_crystal_system      trigonal
_space_group_IT_number           154
_space_group_name_Hall           'P 32 2"'
_space_group_name_H-M_alt        'P 32 2 1'
_symmetry_space_group_name_Hall  'P 32 2"'
_symmetry_space_group_name_H-M   'P 32 2 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-07-10
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_audit_update_record
;
2017-09-06 deposited with the CCDC.
2018-01-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            5
_cell_length_a                   10.6552(4)
_cell_length_b                   10.6552(4)
_cell_length_c                   11.0809(5)
_cell_measurement_reflns_used    1103
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.7070
_cell_measurement_theta_min      4.2270
_cell_volume                     1089.50(8)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2083
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     -8.00  79.00   1.00   14.36    --   15.84  37.00 -90.00   87
  2  ω     16.00  42.00   1.00   14.36    --   15.84 -37.00  90.00   26
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0257295000
_diffrn_orient_matrix_UB_12      0.0680848000
_diffrn_orient_matrix_UB_13      -0.0286911000
_diffrn_orient_matrix_UB_21      0.0089268000
_diffrn_orient_matrix_UB_22      -0.0293540000
_diffrn_orient_matrix_UB_23      -0.0545875000
_diffrn_orient_matrix_UB_31      -0.0718975000
_diffrn_orient_matrix_UB_32      -0.0204008000
_diffrn_orient_matrix_UB_33      -0.0170221000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0216
_diffrn_reflns_av_unetI/netI     0.0432
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            2221
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.995
_diffrn_reflns_theta_min         3.825
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.321
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91265
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    2.107
_exptl_crystal_F_000             681
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.228
_refine_diff_density_min         -0.240
_refine_diff_density_rms         0.061
_refine_ls_abs_structure_details
;
 Flack x determined using 474 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.01(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     107
_refine_ls_number_reflns         1289
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0339
_refine_ls_R_factor_gt           0.0291
_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)+(0.0313P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0617
_refine_ls_wR_factor_ref         0.0648
_reflns_Friedel_coverage         0.712
_reflns_Friedel_fraction_full    0.978
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                1200
_reflns_number_total             1289
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7dt04112h2.cif
_cod_data_source_block           exp_40340
_cod_depositor_comments
'Adding full bibliography for 7045235--7045236.cif.'
_cod_original_cell_volume        1089.50(10)
_cod_original_formula_sum        'C3.60 H4.20 Mn1.20 O8.40 Ti0.60'
_cod_database_code               7045236
_shelxl_version_number           2014-3
_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 99.49
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2. Others
 Fixed Sof: H009(0.5)
3.a Rotating group:
 O009(H009)
3.b Aromatic/amide H refined with riding coordinates:
 C00B(H00B), C00C(H00C), C00D(H00D)
;
_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 1.171
_oxdiff_exptl_absorpt_empirical_full_min 0.865
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z+2/3'
'-x+y, -x, z+1/3'
'y, x, -z'
'x-y, -y, -z+1/3'
'-x, -x+y, -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
Mn01 Mn 0.92259(8) 0.73663(8) 0.48020(6) 0.0226(2) Uani 1 1 d . . .
Ti02 Ti 1.0000 0.50544(11) 0.3333 0.0237(3) Uani 1 2 d S T P
O003 O 1.0000 0.6673(5) 0.3333 0.0245(10) Uani 1 2 d S T P
O004 O 0.8417(4) 0.8228(4) 0.6208(3) 0.0248(8) Uani 1 1 d . . .
O005 O 0.8141(4) 0.8718(4) 0.8103(3) 0.0295(9) Uani 1 1 d . . .
O006 O 1.0504(4) 0.5040(4) 0.5089(3) 0.0358(10) Uani 1 1 d . . .
O007 O 1.0021(4) 0.6518(4) 0.6153(3) 0.0369(9) Uani 1 1 d . . .
O008 O 0.7882(4) 0.3845(4) 0.3762(3) 0.0377(10) Uani 1 1 d . . .
O009 O 1.0000 0.3049(5) 0.3333 0.0380(14) Uani 1 2 d S T P
H009 H 0.9568 0.2532 0.3981 0.057 Uiso 0.5 1 d GR . .
O00A O 0.7245(4) 0.5319(4) 0.4680(4) 0.0430(11) Uani 1 1 d . . .
C00B C 1.0457(6) 0.5654(6) 0.6047(5) 0.0318(13) Uani 1 1 d . . .
H00B H 1.0787 0.5429 0.6745 0.038 Uiso 1 1 calc R . .
C00C C 0.8409(6) 0.8049(6) 0.7333(4) 0.0269(12) Uani 1 1 d . . .
H00C H 0.8624 0.7352 0.7606 0.032 Uiso 1 1 calc R . .
C00D C 0.7000(6) 0.4164(6) 0.4234(5) 0.0380(14) Uani 1 1 d . . .
H00D H 0.6037 0.3426 0.4244 0.046 Uiso 1 1 calc R . .
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 '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'
H H 0.0000 0.0000 '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
O003 Mn01 O004 99.11(12) . 4_556
O003 Mn01 O004 174.71(14) . .
O003 Mn01 O005 88.14(12) . 2_764
O003 Mn01 O007 94.88(13) . .
O003 Mn01 O00A 87.36(13) . .
O004 Mn01 O004 75.93(13) . 4_556
O005 Mn01 O004 88.77(14) 2_764 4_556
O005 Mn01 O004 89.90(14) 2_764 .
O007 Mn01 O004 90.07(13) . .
O007 Mn01 O004 166.00(12) . 4_556
O007 Mn01 O005 91.43(15) . 2_764
O007 Mn01 O00A 90.61(16) . .
O00A Mn01 O004 94.43(15) . .
O00A Mn01 O004 90.30(16) . 4_556
O00A Mn01 O005 175.20(13) . 2_764
O003 Ti02 O006 98.07(11) . 6_765
O003 Ti02 O006 98.07(11) . .
O003 Ti02 O008 94.55(11) . 6_765
O003 Ti02 O008 94.55(11) . .
O003 Ti02 O009 180.0 . .
O006 Ti02 O006 163.9(2) 6_765 .
O006 Ti02 O009 81.93(11) 6_765 .
O006 Ti02 O009 81.93(11) . .
O008 Ti02 O006 89.14(16) 6_765 6_765
O008 Ti02 O006 89.58(16) . 6_765
O008 Ti02 O006 89.14(16) . .
O008 Ti02 O006 89.58(16) 6_765 .
O008 Ti02 O008 170.9(2) 6_765 .
O008 Ti02 O009 85.45(11) 6_765 .
O008 Ti02 O009 85.45(11) . .
Mn01 O003 Mn01 114.1(2) 6_765 .
Ti02 O003 Mn01 122.93(11) . 6_765
Ti02 O003 Mn01 122.93(11) . .
Mn01 O004 Mn01 104.05(13) . 4_556
C00C O004 Mn01 127.7(3) . 4_556
C00C O004 Mn01 127.9(3) . .
C00C O005 Mn01 134.8(3) . 3_675
C00B O006 Ti02 136.6(3) . .
C00B O007 Mn01 129.1(3) . .
C00D O008 Ti02 132.2(4) . .
Ti02 O009 H009 111.3 . .
C00D O00A Mn01 130.6(4) . .
O006 C00B H00B 116.6 . .
O007 C00B O006 126.8(5) . .
O007 C00B H00B 116.6 . .
O004 C00C H00C 117.2 . .
O005 C00C O004 125.6(5) . .
O005 C00C H00C 117.2 . .
O008 C00D H00D 115.7 . .
O00A C00D O008 128.6(5) . .
O00A C00D H00D 115.7 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn01 O003 2.117(3) .
Mn01 O004 2.192(3) .
Mn01 O004 2.197(3) 4_556
Mn01 O005 2.192(4) 2_764
Mn01 O007 2.131(3) .
Mn01 O00A 2.151(4) .
Ti02 O003 1.725(5) .
Ti02 O006 2.020(4) 6_765
Ti02 O006 2.020(4) .
Ti02 O008 2.018(4) .
Ti02 O008 2.018(4) 6_765
Ti02 O009 2.137(5) .
O003 Mn01 2.117(3) 6_765
O004 Mn01 2.197(3) 4_556
O004 C00C 1.260(5) .
O005 Mn01 2.192(4) 3_675
O005 C00C 1.234(5) .
O006 C00B 1.261(6) .
O007 C00B 1.226(7) .
O008 C00D 1.261(7) .
O009 H009 0.8815 .
O00A C00D 1.228(7) .
C00B H00B 0.9300 .
C00C H00C 0.9300 .
C00D H00D 0.9300 .
