#------------------------------------------------------------------------------
#$Date: 2019-11-17 12:10:56 +0200 (Sun, 17 Nov 2019) $
#$Revision: 229799 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/52/7045235.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_7045235
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           152
_space_group_name_Hall           'P 31 2"'
_space_group_name_H-M_alt        'P 31 2 1'
_symmetry_space_group_name_Hall  'P 31 2"'
_symmetry_space_group_name_H-M   'P 31 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                   10.6510(3)
_cell_length_b                   10.6510(3)
_cell_length_c                   11.0943(3)
_cell_measurement_reflns_used    1642
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.4710
_cell_measurement_theta_min      4.2260
_cell_volume                     1089.96(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_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_area_resol_mean 16.2083
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -50.00   53.00   0.2500   13.2450
omega____ theta____ kappa____ phi______ frames
    -       15.8360  -19.0000    0.0000 412
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0561008000
_diffrn_orient_matrix_UB_12      0.0725658000
_diffrn_orient_matrix_UB_13      -0.0093628000
_diffrn_orient_matrix_UB_21      0.0224350000
_diffrn_orient_matrix_UB_22      0.0038702000
_diffrn_orient_matrix_UB_23      0.0607508000
_diffrn_orient_matrix_UB_31      0.0475685000
_diffrn_orient_matrix_UB_32      -0.0251745000
_diffrn_orient_matrix_UB_33      -0.0176380000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0170
_diffrn_reflns_av_unetI/netI     0.0306
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            2056
_diffrn_reflns_point_group_measured_fraction_full 0.967
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.994
_diffrn_reflns_theta_min         3.826
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.320
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91221
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
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         0.267
_refine_diff_density_min         -0.188
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details
;
 Flack x determined using 493 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.056(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     107
_refine_ls_number_reflns         1275
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0230
_refine_ls_R_factor_gt           0.0215
_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)+(0.0247P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0511
_refine_ls_wR_factor_ref         0.0517
_reflns_Friedel_coverage         0.693
_reflns_Friedel_fraction_full    0.953
_reflns_Friedel_fraction_max     0.970
_reflns_number_gt                1220
_reflns_number_total             1275
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7dt04112h2.cif
_cod_data_source_block           exp_40441
_cod_depositor_comments
'Adding full bibliography for 7045235--7045236.cif.'
_cod_original_cell_volume        1089.96(7)
_cod_original_formula_sum        'C3.60 H4.20 Mn1.20 O8.40 Ti0.60'
_cod_database_code               7045235
_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: H007(0.5)
3.a Rotating group:
 O007(H007)
3.b Aromatic/amide H refined with riding coordinates:
 C00B(H00B), C00C(H00C), C00D(H00D)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z+1/3'
'-x+y, -x, z+2/3'
'y, x, -z'
'x-y, -y, -z+2/3'
'-x, -x+y, -z+1/3'
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 0.92250(6) 0.18597(6) 0.31344(4) 0.02365(17) Uani 1 1 d . . .
Ti02 Ti 1.0000 0.49476(9) 0.1667 0.0243(2) Uani 1 2 d S T P
O003 O 1.0000 0.3327(4) 0.1667 0.0264(8) Uani 1 2 d S T P
O004 O 0.8415(3) 0.0189(3) 0.4541(2) 0.0251(6) Uani 1 1 d . . .
O005 O 1.0501(3) 0.5462(3) 0.3422(2) 0.0354(7) Uani 1 1 d . . .
O006 O 0.8142(3) -0.0578(3) 0.6436(2) 0.0303(7) Uani 1 1 d . . .
O007 O 1.0000 0.6948(4) 0.1667 0.0383(11) Uani 1 2 d S T P
H007 H 1.0443 0.7554 0.0976 0.057 Uiso 0.5 1 d GR . .
O008 O 1.0017(3) 0.3496(3) 0.4484(2) 0.0398(7) Uani 1 1 d . . .
O009 O 0.7873(3) 0.4027(3) 0.2096(3) 0.0396(7) Uani 1 1 d . . .
O00A O 0.7244(3) 0.1929(4) 0.3014(3) 0.0452(8) Uani 1 1 d . . .
C00B C 1.0453(4) 0.4804(5) 0.4383(3) 0.0322(9) Uani 1 1 d . . .
H00B H 1.0777 0.5358 0.5082 0.039 Uiso 1 1 calc R . .
C00C C 0.8409(5) 0.0357(4) 0.5661(3) 0.0274(9) Uani 1 1 d . . .
H00C H 0.8625 0.1270 0.5933 0.033 Uiso 1 1 calc R . .
C00D C 0.6996(5) 0.2834(5) 0.2564(4) 0.0398(10) Uani 1 1 d . . .
H00D H 0.6032 0.2606 0.2572 0.048 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 99.08(9) . 5
O003 Mn01 O004 174.75(11) . .
O003 Mn01 O006 88.14(9) . 3_764
O003 Mn01 O008 95.05(10) . .
O003 Mn01 O00A 87.37(10) . .
O004 Mn01 O004 76.00(9) . 5
O006 Mn01 O004 88.79(11) 3_764 5
O006 Mn01 O004 89.92(10) 3_764 .
O008 Mn01 O004 165.87(9) . 5
O008 Mn01 O004 89.87(10) . .
O008 Mn01 O006 91.43(11) . 3_764
O008 Mn01 O00A 90.55(12) . .
O00A Mn01 O004 90.34(12) . 5
O00A Mn01 O004 94.43(11) . .
O00A Mn01 O006 175.23(10) . 3_764
O003 Ti02 O005 98.00(8) . 6_765
O003 Ti02 O005 98.00(8) . .
O003 Ti02 O007 180.0 . .
O003 Ti02 O009 94.30(8) . 6_765
O003 Ti02 O009 94.30(8) . .
O005 Ti02 O005 164.01(16) . 6_765
O005 Ti02 O007 82.00(8) . .
O005 Ti02 O007 82.00(8) 6_765 .
O005 Ti02 O009 89.69(12) 6_765 .
O005 Ti02 O009 89.11(12) . .
O005 Ti02 O009 89.11(12) 6_765 6_765
O005 Ti02 O009 89.69(12) . 6_765
O009 Ti02 O007 85.70(8) 6_765 .
O009 Ti02 O007 85.70(8) . .
O009 Ti02 O009 171.40(16) 6_765 .
Mn01 O003 Mn01 114.21(18) . 6_765
Ti02 O003 Mn01 122.90(9) . .
Ti02 O003 Mn01 122.89(9) . 6_765
Mn01 O004 Mn01 103.98(9) . 5
C00C O004 Mn01 128.0(2) . .
C00C O004 Mn01 127.6(2) . 5
C00B O005 Ti02 137.0(3) . .
C00C O006 Mn01 134.6(2) . 2_645
Ti02 O007 H007 115.3 . .
C00B O008 Mn01 129.2(3) . .
C00D O009 Ti02 132.5(3) . .
C00D O00A Mn01 130.7(3) . .
O005 C00B H00B 116.9 . .
O008 C00B O005 126.3(4) . .
O008 C00B H00B 116.9 . .
O004 C00C H00C 117.0 . .
O006 C00C O004 126.0(4) . .
O006 C00C H00C 117.0 . .
O009 C00D H00D 115.8 . .
O00A C00D O009 128.4(4) . .
O00A C00D H00D 115.8 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn01 O003 2.118(2) .
Mn01 O004 2.194(2) .
Mn01 O004 2.197(3) 5
Mn01 O006 2.189(3) 3_764
Mn01 O008 2.127(3) .
Mn01 O00A 2.152(3) .
Ti02 O003 1.726(4) .
Ti02 O005 2.021(3) 6_765
Ti02 O005 2.021(3) .
Ti02 O007 2.131(4) .
Ti02 O009 2.024(3) 6_765
Ti02 O009 2.024(3) .
O003 Mn01 2.118(2) 6_765
O004 Mn01 2.197(3) 5
O004 C00C 1.255(4) .
O005 C00B 1.263(5) .
O006 Mn01 2.189(3) 2_645
O006 C00C 1.237(4) .
O007 H007 0.9599 .
O008 C00B 1.233(5) .
O009 C00D 1.253(5) .
O00A C00D 1.226(5) .
C00B H00B 0.9300 .
C00C H00C 0.9300 .
C00D H00D 0.9300 .
