Three unprecedent polycational templated cuprous thiocyanate networks: synthesis, structure, and properties
Li, Li; Zhu, Lu; Yue, Zhong-Cheng; Zhang, Wen-Li; Zhang, Bing; Niu, Yun-Yin; Hou, Hong-Wei; CrystEngComm 15 (2013) 8395–; doi:10.1039/c3ce41430b

data_7211192
_publ_section_title
;
 Three unprecedent polycational templated cuprous thiocyanate networks:
 synthesis, structure, and properties
;
_journal_issue                   42
_journal_name_full               CrystEngComm
_journal_page_first              8395
_journal_paper_doi               10.1039/c3ce41430b
_journal_volume                  15
_journal_year                    2013
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C5 Cu2 N5 S5, C27 H30 N3'
_chemical_formula_sum            'C32 H30 Cu2 N8 S5'
_chemical_formula_weight         814.02
_chemical_name_systematic
;
?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-12-26
_audit_creation_method
;
Olex2 1.2
(compiled Dec 5 2012 16:20:19, GUI svn.r4385)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 91.532(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.6275(2)
_cell_length_b                   9.2206(2)
_cell_length_c                   19.3389(4)
_cell_measurement_reflns_used    3384
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      26.3146
_cell_measurement_theta_min      2.9406
_cell_volume                     1716.13(6)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      291.15
_diffrn_detector_area_resol_mean 16.2312
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
1 omega -7.00 19.00 1.0000 20.0000
omega____ theta____ kappa____ phi______ frames
- -17.1323 -99.0000 0.0000 26

2 omega -17.00 34.00 1.0000 20.0000
omega____ theta____ kappa____ phi______ frames
- 19.7104 -57.0000 -150.0000 51

3 omega -36.00 25.00 1.0000 20.0000
omega____ theta____ kappa____ phi______ frames
- 19.7104 -57.0000 0.0000 61

4 omega -49.00 50.00 1.0000 20.0000
omega____ theta____ kappa____ phi______ frames
- 19.7104 -77.0000 150.0000 99
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0132329000
_diffrn_orient_matrix_UB_12      0.0558055000
_diffrn_orient_matrix_UB_13      0.0245443000
_diffrn_orient_matrix_UB_21      0.0073819000
_diffrn_orient_matrix_UB_22      -0.0527178000
_diffrn_orient_matrix_UB_23      0.0265430000
_diffrn_orient_matrix_UB_31      0.0721518000
_diffrn_orient_matrix_UB_32      -0.0047960000
_diffrn_orient_matrix_UB_33      -0.0062118000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0203
_diffrn_reflns_av_unetI/netI     0.0428
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            7781
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.95
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_source_current           n/a
_diffrn_source_voltage           n/a
_exptl_absorpt_coefficient_mu    1.581
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.99346
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.575
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.296
_refine_diff_density_min         -0.323
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.021(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     427
_refine_ls_number_reflns         5396
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0448
_refine_ls_R_factor_gt           0.0344
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0299P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0651
_refine_ls_wR_factor_ref         0.0691
_reflns_number_gt                4647
_reflns_number_total             5396
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce41430b.txt
_cod_data_source_block           nyy2012121803
_cod_original_cell_volume        1716.13(7)
_cod_database_code               7211192
_chemical_oxdiff_formula         C20H20N4O4Cu1S1
_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:
H20 of C20, H22 of C22, H19 of C19, {H14A,H14B} of C14, H21 of C21, H25 of
C25, H29 of C29, {H16A,H16B} of C16, {H12A,H12B} of C12, H32 of C32, H26 of
C26, H24 of C24, H27 of C27, H23 of C23, H30 of C30, H28 of C28, H18 of C18,
H31 of C31
At 1.5 times of:
{H13A,H13B,H13C} of C13, {H15A,H15B,H15C} of C15, {H17A,H17B,H17C} of C17
2.a Secondary CH2 refined with riding coordinates:
C12(H12A,H12B), C14(H14A,H14B), C16(H16A,H16B)
2.b Aromatic/amide H refined with riding coordinates:
C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24),
C25(H25), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32)
2.c Idealised Me refined as rotating group:
C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C)
;