#------------------------------------------------------------------------------
#$Date: 2020-04-04 07:13:48 +0300 (Sat, 04 Apr 2020) $
#$Revision: 250070 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/43/4134375.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_4134375
loop_
_publ_author_name
'Sorolla, 2nd, Maurice'
'Wang, Xiqu'
'Koo, Hyun-Joo'
'Whangbo, Myung-Hwan'
'Jacobson, Allan J.'
_publ_section_title
;
 Synthesis of the Elusive S = ¹/₂ Star
 Structure: A Possible Quantum Spin Liquid Candidate.
;
_journal_issue                   11
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5013
_journal_page_last               5016
_journal_paper_doi               10.1021/jacs.0c00901
_journal_volume                  142
_journal_year                    2020
_chemical_formula_sum            'C12 H50 Cu6 N6 O34.47 S8'
_chemical_formula_weight         1467.88
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   12.723(3)
_cell_length_b                   12.723(3)
_cell_length_c                   25.810(7)
_cell_measurement_reflns_used    9857
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      28.42
_cell_measurement_theta_min      2.44
_cell_volume                     3618.2(16)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'narrow frame ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0218
_diffrn_reflns_av_unetI/netI     0.0352
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.944
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            2408
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.944
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.211
_diffrn_reflns_theta_min         2.431
_exptl_absorpt_coefficient_mu    3.047
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5522
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.021
_exptl_crystal_description       plate
_exptl_crystal_F_000             2225
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.643
_refine_diff_density_min         -0.755
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.223
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     136
_refine_ls_number_reflns         1707
_refine_ls_number_restraints     68
_refine_ls_restrained_S_all      1.200
_refine_ls_R_factor_all          0.0288
_refine_ls_R_factor_gt           0.0258
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0249P)²+4.9908P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0686
_refine_ls_wR_factor_ref         0.0699
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1572
_reflns_number_total             1707
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja0c00901_si_002.cif
_cod_data_source_block           MS691
_cod_depositor_comments          'Adding full bibliography for 4134375.cif.'
_cod_original_cell_volume        3618(2)
_cod_database_code               4134375
_shelx_shelxl_version_number     2018/3
_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.
;
_shelx_estimated_absorpt_t_min   0.424
_shelx_estimated_absorpt_t_max   0.863
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.84531(2) 0.85782(2) 0.30974(2) 0.01134(11) Uani 1 1 d . . . . .
S1 S 0.57420(5) 0.67687(5) 0.29103(2) 0.01275(14) Uani 1 1 d . . . . .
S2 S 1.000000 1.000000 0.21678(4) 0.0139(2) Uani 1 3 d S T P . .
O1 O 1.000000 1.000000 0.33186(11) 0.0112(5) Uani 1 3 d DS T P . .
H1 H 1.000000 1.000000 0.3635(8) 0.013 Uiso 1 3 d DS U P . .
O2 O 1.000000 1.000000 0.16076(12) 0.0228(7) Uani 1 3 d S T P . .
O3 O 0.89571(15) 0.88509(15) 0.23673(7) 0.0189(4) Uani 1 1 d . . . . .
O4 O 0.70324(15) 0.71015(15) 0.28760(8) 0.0243(4) Uani 1 1 d . . . . .
O5 O 0.56760(14) 0.79129(14) 0.29369(6) 0.0157(4) Uani 1 1 d . . . . .
O6 O 0.50810(18) 0.60617(17) 0.24603(7) 0.0266(4) Uani 1 1 d . . . . .
O7 O 0.52189(15) 0.60792(16) 0.33925(7) 0.0181(4) Uani 1 1 d . . . . .
N1_1 N 0.3840(16) 0.3544(16) 0.2468(7) 0.016(2) Uani 0.5 1 d D U P A 1
H1A_1 H 0.324892 0.325379 0.271444 0.019 Uiso 0.5 1 calc R U P A 1
H1AB_1 H 0.419104 0.436712 0.246516 0.019 Uiso 0.5 1 calc R U P A 1
C1_1 C 0.3275(19) 0.3069(19) 0.1958(9) 0.038(3) Uani 0.5 1 d D U P A 1
H1B_1 H 0.390796 0.333993 0.169267 0.057 Uiso 0.5 1 calc R U P A 1
H1C_1 H 0.272173 0.337151 0.187487 0.057 Uiso 0.5 1 calc R U P A 1
H1D_1 H 0.281941 0.217998 0.196909 0.057 Uiso 0.5 1 calc R U P A 1
C2_1 C 0.4768(16) 0.322(2) 0.2613(5) 0.036(3) Uani 0.5 1 d D U P A 1
H2A_1 H 0.440489 0.233349 0.260544 0.054 Uiso 0.5 1 calc R U P A 1
H2B_1 H 0.506912 0.351896 0.296196 0.054 Uiso 0.5 1 calc R U P A 1
H2C_1 H 0.544252 0.358588 0.236568 0.054 Uiso 0.5 1 calc R U P A 1
N1_2 N 0.3719(19) 0.351(2) 0.2401(8) 0.027(4) Uani 0.5 1 d D U P B 2
H1A_2 H 0.316264 0.316636 0.265984 0.032 Uiso 0.5 1 calc R U P B 2
H1AB_2 H 0.411903 0.432354 0.244899 0.032 Uiso 0.5 1 calc R U P B 2
C1_2 C 0.307(2) 0.323(2) 0.1904(9) 0.046(4) Uani 0.5 1 d D U P B 2
H1B_2 H 0.364347 0.341195 0.161879 0.069 Uiso 0.5 1 calc R U P B 2
H1C_2 H 0.268375 0.372982 0.186773 0.069 Uiso 0.5 1 calc R U P B 2
H1D_2 H 0.244526 0.237086 0.189328 0.069 Uiso 0.5 1 calc R U P B 2
C2_2 C 0.4606(18) 0.308(2) 0.2452(6) 0.044(4) Uani 0.5 1 d D U P B 2
H2A_2 H 0.418433 0.219224 0.241593 0.066 Uiso 0.5 1 calc R U P B 2
H2B_2 H 0.499481 0.330705 0.279329 0.066 Uiso 0.5 1 calc R U P B 2
H2C_2 H 0.522474 0.344980 0.218123 0.066 Uiso 0.5 1 calc R U P B 2
O8 O 1.000000 1.000000 0.4419(7) 0.054(8) Uani 0.237(16) 3 d S T P . .
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'
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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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
_geom_angle_publ_flag
O4 Cu1 O3 87.25(8) . . ?
O4 Cu1 O1 174.16(5) . . ?
O3 Cu1 O1 91.59(9) . . ?
O4 Cu1 O5 94.05(7) . 16_665 ?
O3 Cu1 O5 154.92(7) . 16_665 ?
O1 Cu1 O5 89.43(8) . 16_665 ?
O4 Cu1 O7 90.21(7) . 17 ?
O3 Cu1 O7 94.18(7) . 17 ?
O1 Cu1 O7 84.16(5) . 17 ?
O5 Cu1 O7 110.85(7) 16_665 17 ?
O6 S1 O7 110.92(11) . . ?
O6 S1 O4 110.21(12) . . ?
O7 S1 O4 109.08(11) . . ?
O6 S1 O5 109.96(11) . . ?
O7 S1 O5 108.10(10) . . ?
O4 S1 O5 108.51(10) . . ?
O2 S2 O3 110.20(7) . . ?
O2 S2 O3 110.20(7) . 2_765 ?
O3 S2 O3 108.73(8) . 2_765 ?
O2 S2 O3 110.20(7) . 3_675 ?
O3 S2 O3 108.73(8) . 3_675 ?
O3 S2 O3 108.73(8) 2_765 3_675 ?
Cu1 O1 Cu1 112.02(7) . 3_675 ?
Cu1 O1 Cu1 112.02(7) . 2_765 ?
Cu1 O1 Cu1 112.02(7) 3_675 2_765 ?
Cu1 O1 H1 106.78(8) . . ?
Cu1 O1 H1 106.78(8) 3_675 . ?
Cu1 O1 H1 106.78(8) 2_765 . ?
S2 O3 Cu1 123.80(10) . . ?
S1 O4 Cu1 128.75(10) . . ?
S1 O5 Cu1 115.11(9) . 16_665 ?
S1 O7 Cu1 122.89(10) . 18_545 ?
C1_1 N1_1 C2_1 113.7(11) . . ?
C1_1 N1_1 H1A_1 108.8 . . ?
C2_1 N1_1 H1A_1 108.8 . . ?
C1_1 N1_1 H1AB_1 108.8 . . ?
C2_1 N1_1 H1AB_1 108.8 . . ?
H1A_1 N1_1 H1AB_1 107.7 . . ?
N1_1 C1_1 H1B_1 109.5 . . ?
N1_1 C1_1 H1C_1 109.5 . . ?
H1B_1 C1_1 H1C_1 109.5 . . ?
N1_1 C1_1 H1D_1 109.5 . . ?
H1B_1 C1_1 H1D_1 109.5 . . ?
H1C_1 C1_1 H1D_1 109.5 . . ?
N1_1 C2_1 H2A_1 109.5 . . ?
N1_1 C2_1 H2B_1 109.5 . . ?
H2A_1 C2_1 H2B_1 109.5 . . ?
N1_1 C2_1 H2C_1 109.5 . . ?
H2A_1 C2_1 H2C_1 109.5 . . ?
H2B_1 C2_1 H2C_1 109.5 . . ?
C1_2 N1_2 C2_2 115.6(12) . . ?
C1_2 N1_2 H1A_2 108.4 . . ?
C2_2 N1_2 H1A_2 108.4 . . ?
C1_2 N1_2 H1AB_2 108.4 . . ?
C2_2 N1_2 H1AB_2 108.4 . . ?
H1A_2 N1_2 H1AB_2 107.4 . . ?
N1_2 C1_2 H1B_2 109.5 . . ?
N1_2 C1_2 H1C_2 109.5 . . ?
H1B_2 C1_2 H1C_2 109.5 . . ?
N1_2 C1_2 H1D_2 109.5 . . ?
H1B_2 C1_2 H1D_2 109.5 . . ?
H1C_2 C1_2 H1D_2 109.5 . . ?
N1_2 C2_2 H2A_2 109.5 . . ?
N1_2 C2_2 H2B_2 109.5 . . ?
H2A_2 C2_2 H2B_2 109.5 . . ?
N1_2 C2_2 H2C_2 109.5 . . ?
H2A_2 C2_2 H2C_2 109.5 . . ?
H2B_2 C2_2 H2C_2 109.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O4 1.9307(18) . ?
Cu1 O3 1.9647(18) . ?
Cu1 O1 1.9777(10) . ?
Cu1 O5 1.9911(17) 16_665 ?
Cu1 O7 2.2627(18) 17 ?
S1 O6 1.4523(19) . ?
S1 O7 1.4755(18) . ?
S1 O4 1.4790(17) . ?
S1 O5 1.5011(17) . ?
S2 O2 1.446(3) . ?
S2 O3 1.4910(17) . ?
S2 O3 1.4911(17) 2_765 ?
S2 O3 1.4911(17) 3_675 ?
O1 H1 0.817(19) . ?
N1_1 C1_1 1.476(11) . ?
N1_1 C2_1 1.481(11) . ?
N1_1 H1A_1 0.9100 . ?
N1_1 H1AB_1 0.9100 . ?
C1_1 H1B_1 0.9800 . ?
C1_1 H1C_1 0.9800 . ?
C1_1 H1D_1 0.9800 . ?
C2_1 H2A_1 0.9800 . ?
C2_1 H2B_1 0.9800 . ?
C2_1 H2C_1 0.9800 . ?
N1_2 C1_2 1.472(11) . ?
N1_2 C2_2 1.483(11) . ?
N1_2 H1A_2 0.9100 . ?
N1_2 H1AB_2 0.9100 . ?
C1_2 H1B_2 0.9800 . ?
C1_2 H1C_2 0.9800 . ?
C1_2 H1D_2 0.9800 . ?
C2_2 H2A_2 0.9800 . ?
C2_2 H2B_2 0.9800 . ?
C2_2 H2C_2 0.9800 . ?
