#------------------------------------------------------------------------------
#$Date: 2021-06-02 10:43:30 +0300 (Wed, 02 Jun 2021) $
#$Revision: 265667 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/30/1563077.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_1563077
loop_
_publ_author_name
'Fomina, Irina'
'Dobrokhotova, Zhanna'
'Aleksandrov, Grygory'
'Emelina, Anna'
'Bykov, Mikhail'
'Malkerova, Irina'
'Bogomyakov, Artem'
'Puntus, Lada'
'Novotortsev, Vladimir'
'Eremenko, Igor'
_publ_section_title
;
 Novel 1D coordination polymer {Tm(Piv)3}n: Synthesis, structure, magnetic
 properties and thermal behavior
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              49
_journal_page_last               55
_journal_paper_doi               10.1016/j.jssc.2011.09.033
_journal_volume                  185
_journal_year                    2012
_chemical_formula_moiety         'C15 H27 O6 Tm'
_chemical_formula_sum            'C15 H27 O6 Tm'
_chemical_formula_weight         472.30
_space_group_IT_number           165
_space_group_name_Hall           '-P 3 2"c'
_space_group_name_H-M_alt        'P -3 c 1'
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-P 3 2"c'
_symmetry_space_group_name_H-M   'P -3 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   10.7469(7)
_cell_length_b                   10.7469(7)
_cell_length_c                   9.5447(7)
_cell_measurement_temperature    150(2)
_cell_volume                     954.68(11)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Smart CCD ApexII'
_diffrn_measurement_method       /w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0430
_diffrn_reflns_av_sigmaI/netI    0.0177
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            9269
_diffrn_reflns_theta_full        28.27
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         2.19
_exptl_absorpt_coefficient_mu    4.668
_exptl_absorpt_correction_T_max  0.8001
_exptl_absorpt_correction_T_min  0.4870
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2004/1, Sheldrick, G.M., (2004)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.643
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelogram
_exptl_crystal_F_000             468
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.614
_refine_diff_density_min         -2.354
_refine_diff_density_rms         0.261
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     49
_refine_ls_number_reflns         796
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0671
_refine_ls_R_factor_gt           0.0552
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1000P)²+30.5000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1672
_refine_ls_wR_factor_ref         0.1778
_reflns_number_gt                603
_reflns_number_total             796
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            JSSC-2012-185-49.cif
_cod_data_source_block           tm
_cod_original_sg_symbol_H-M      P-3c1
_cod_database_code               1563077
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'y, x, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-y, -x, 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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Tm1 Tm 0.0000 0.0000 0.0000 0.0187(4) Uani 1 6 d S . .
O1 O 0.1648(16) 0.001(2) 0.1332(8) 0.102(7) Uani 1 1 d D . .
C1 C 0.2088(12) 0.0000 0.2500 0.042(4) Uani 1 2 d SD . .
C2 C 0.3456(13) 0.0000 0.2500 0.048(5) Uani 1 2 d SD . .
C3 C 0.341(5) -0.097(4) 0.127(3) 0.11(2) Uani 0.50 1 d PD A 1
H3A H 0.2812 -0.1980 0.1537 0.162 Uiso 0.50 1 calc PR A 1
H3B H 0.4391 -0.0770 0.1072 0.162 Uiso 0.50 1 calc PR A 1
H3C H 0.3013 -0.0767 0.0440 0.162 Uiso 0.50 1 calc PR A 1
C4 C 0.430(3) 0.074(5) 0.115(2) 0.17(4) Uani 0.50 1 d PD A 2
H4A H 0.4785 0.1788 0.1261 0.249 Uiso 0.50 1 calc PR A 2
H4B H 0.3639 0.0453 0.0352 0.249 Uiso 0.50 1 calc PR A 2
H4C H 0.5024 0.0455 0.0970 0.249 Uiso 0.50 1 calc PR A 2
C5 C 0.4972(15) 0.125(2) 0.263(3) 0.055(8) Uani 0.50 1 d PD A 3
H5A H 0.5015 0.1886 0.3388 0.082 Uiso 0.50 1 calc PR A 3
H5B H 0.5250 0.1794 0.1744 0.082 Uiso 0.50 1 calc PR A 3
H5C H 0.5631 0.0897 0.2827 0.082 Uiso 0.50 1 calc PR A 3
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
Tm1 0.0229(4) 0.0229(4) 0.0104(5) 0.000 0.000 0.0115(2)
O1 0.088(9) 0.27(2) 0.016(4) 0.003(8) -0.002(5) 0.142(14)
C1 0.039(7) 0.067(14) 0.031(8) 0.001(8) 0.001(4) 0.033(7)
C2 0.041(6) 0.094(17) 0.026(7) 0.008(9) 0.004(5) 0.047(9)
C3 0.22(7) 0.13(4) 0.07(3) 0.01(3) 0.03(3) 0.16(5)
C4 0.019(15) 0.29(9) 0.07(3) 0.01(4) 0.021(17) -0.01(3)
C5 0.045(16) 0.07(2) 0.08(2) 0.031(17) 0.020(15) 0.050(16)
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tm Tm -0.3139 5.2483 '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
O1 Tm1 O1 90.7(3) 7 3
O1 Tm1 O1 89.3(3) 7 8
O1 Tm1 O1 90.7(3) 3 8
O1 Tm1 O1 89.3(3) 7 9
O1 Tm1 O1 179.999(1) 3 9
O1 Tm1 O1 89.3(3) 8 9
O1 Tm1 O1 179.999(1) 7 .
O1 Tm1 O1 89.3(3) 3 .
O1 Tm1 O1 90.7(3) 8 .
O1 Tm1 O1 90.7(3) 9 .
O1 Tm1 O1 90.7(3) 7 2
O1 Tm1 O1 89.3(3) 3 2
O1 Tm1 O1 179.999(2) 8 2
O1 Tm1 O1 90.7(3) 9 2
O1 Tm1 O1 89.3(3) . 2
C1 O1 Tm1 148.9(9) . .
O1 C1 O1 133.6(15) . 4
O1 C1 C2 113.2(7) . .
O1 C1 C2 113.2(7) 4 .
C1 C2 C5 129.1(10) . 4
C1 C2 C5 129.1(10) . .
C5 C2 C5 102(2) 4 .
C1 C2 C3 107.8(15) . .
C5 C2 C3 45.5(16) 4 .
C5 C2 C3 108(2) . .
C1 C2 C3 107.8(15) . 4
C5 C2 C3 108(2) 4 4
C5 C2 C3 45.5(16) . 4
C3 C2 C3 144(3) . 4
C1 C2 C4 109.3(15) . 4
C5 C2 C4 60.9(14) 4 4
C5 C2 C4 94(2) . 4
C3 C2 C4 105.5(15) . 4
C3 C2 C4 62.0(15) 4 4
C1 C2 C4 109.3(15) . .
C5 C2 C4 94(2) 4 .
C5 C2 C4 60.9(14) . .
C3 C2 C4 62.0(15) . .
C3 C2 C4 105.5(15) 4 .
C4 C2 C4 141(3) 4 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Tm1 O1 2.176(8) 7
Tm1 O1 2.176(8) 3
Tm1 O1 2.176(8) 8
Tm1 O1 2.176(8) 9
Tm1 O1 2.176(8) .
Tm1 O1 2.176(8) 2
O1 C1 1.213(7) .
C1 O1 1.213(7) 4
C1 C2 1.470(9) .
C2 C5 1.513(10) 4
C2 C5 1.513(10) .
C2 C3 1.551(10) .
C2 C3 1.551(10) 4
C2 C4 1.553(10) 4
C2 C4 1.553(10) .
