Three cation-templated Cu(i) self-assemblies: synthesis, structures, and photocatalytic properties
Xu, Man-Man; Li, Yao; Zheng, Lin-Jie; Niu, Yun-Yin; Hou, Hong-Wei; New J. Chem. 40 (2016) 6086–; doi:10.1039/C5NJ03321G

data_7055521
_publ_section_title
;
 Three cation-templated Cu(i) self-assemblies: synthesis, structures, and
 photocatalytic properties
;
_journal_issue                   7
_journal_name_full               'New J. Chem.'
_journal_page_first              6086
_journal_paper_doi               10.1039/C5NJ03321G
_journal_volume                  40
_journal_year                    2016
_chemical_formula_moiety         '2(C18 H20 N4), Cu4 I8'
_chemical_formula_sum            'C36 H40 Cu4 I8 N8'
_chemical_formula_weight         1854.12
_space_group_crystal_system      orthorhombic
_space_group_IT_number           63
_space_group_name_Hall           '-C 2c 2'
_space_group_name_H-M_alt        'C m c m'
_symmetry_space_group_name_Hall  '-C 2c 2'
_symmetry_space_group_name_H-M   'C m c m'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_block_doi                 10.5517/ccdc.csd.cc1k1klr
_audit_creation_date             2016-03-24
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-03-28 deposited with the CCDC.
2016-04-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.9299(6)
_cell_length_b                   14.8450(8)
_cell_length_c                   19.6945(8)
_cell_measurement_reflns_used    1718
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      27.7730
_cell_measurement_theta_min      3.5890
_cell_volume                     4949.7(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      291.15
_diffrn_detector_area_resol_mean 16.2312
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega   -7.00   19.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.2885  -99.0000  -30.0000 26

  2 omega  -53.00   65.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7885    0.0000  -60.0000 118
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0187831000
_diffrn_orient_matrix_UB_12      -0.0383544000
_diffrn_orient_matrix_UB_13      -0.0141301000
_diffrn_orient_matrix_UB_21      -0.0024269000
_diffrn_orient_matrix_UB_22      0.0196943000
_diffrn_orient_matrix_UB_23      -0.0327595000
_diffrn_orient_matrix_UB_31      0.0373916000
_diffrn_orient_matrix_UB_32      0.0205069000
_diffrn_orient_matrix_UB_33      0.0050102000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0292
_diffrn_reflns_av_unetI/netI     0.0401
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            6572
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_min         2.933
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.720
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79195
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.488
_exptl_crystal_description       block
_exptl_crystal_F_000             3408
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.875
_refine_diff_density_min         -2.727
_refine_diff_density_rms         0.221
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     143
_refine_ls_number_reflns         2702
_refine_ls_number_restraints     43
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0740
_refine_ls_R_factor_gt           0.0569
_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/[\s^2^(Fo^2^)+(0.0874P)^2^+74.8485P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1578
_refine_ls_wR_factor_ref         0.1712
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2097
_reflns_number_total             2702
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5nj03321g2.cif
_cod_data_source_block           nyy15060203
_cod_depositor_comments
'Adding full bibliography for 7055521--7055522.cif.'
_cod_database_code               7055521
_chemical_oxdiff_formula         C9H9N2I2Cu1
_shelx_estimated_absorpt_t_max   0.378
_shelx_estimated_absorpt_t_min   0.347
_reflns_odcompleteness_completeness 99.72
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
2. Restrained distances
 N1-C5
 1.37 with sigma of 0.02
 N1-C6
 1.37 with sigma of 0.02
 N1-C6A
 1.36 with sigma of 0.02
 C4-C5
 1.38 with sigma of 0.02
 C2-C1
 1.38 with sigma of 0.02
 C6A-C8
 1.55 with sigma of 0.02
 Cu2-I4
 2.3 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C6) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C10) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C1) \\sim Ueq, Uanis(N1) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(I4) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C6) = Uanis(C6A)
4. Others
 Sof(C6A)=Sof(H6AA)=Sof(H6AB)=1-FVAR(1)
 Sof(C6)=Sof(H6A)=Sof(H6B)=FVAR(1)
5.a Riding coordinates:
 C6A(H6AA,H6AB)
5.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B)
5.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C7(H7), C9(H9), C10(H10)
5.d X=CH2 refined with riding coordinates:
 N2(H2A,H2B)
;
_shelx_res_checksum              1598
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'