New copper(I) iodides with bisimidazole molecules: Synthesis, structural characterization and photoluminescence property
Wang, Rong-Yan; Zhang, Xiao; Yang, Qing-Feng; Huo, Qi-Sheng; Yu, Jie-Hui; Xu, Jia-Ning; Xu, Ji-Qing; Journal of Solid State Chemistry 251 (2017) 176–185; doi:10.1016/j.jssc.2017.04.022

data_1560450
_publ_section_title
;
 New copper(I) iodides with bisimidazole molecules: Synthesis, structural
 characterization and photoluminescence property
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              176
_journal_page_last               185
_journal_paper_doi               10.1016/j.jssc.2017.04.022
_journal_volume                  251
_journal_year                    2017
_chemical_formula_moiety         'C28 H35 Cu4 I4 N8'
_chemical_formula_sum            'C28 H35 Cu4 I4 N8'
_chemical_formula_weight         1245.40
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 114.93(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   42.929(9)
_cell_length_b                   9.984(2)
_cell_length_c                   19.943(4)
_cell_measurement_reflns_used    22681
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.73
_cell_measurement_theta_min      2.995
_cell_volume                     7751(3)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0753
_diffrn_reflns_av_unetI/netI     0.0739
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       51
_diffrn_reflns_limit_h_min       -51
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            28754
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         2.995
_exptl_absorpt_coefficient_mu    5.381
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.134
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       clumnar
_exptl_crystal_F_000             4696
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.265
_refine_diff_density_min         -0.913
_refine_diff_density_rms         0.150
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     458
_refine_ls_number_reflns         7038
_refine_ls_number_restraints     75
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0970
_refine_ls_R_factor_gt           0.0595
_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^)+(0.0331P)^2^+53.9965P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1064
_refine_ls_wR_factor_ref         0.1193
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4666
_reflns_number_total             7038
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            mmc4.cif
_cod_data_source_block           4
_cod_database_code               1560450
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C5DA-C3D
 2.51 with sigma of 0.02
 C4DA-C3D
 1.5 with sigma of 0.02
 C5DA-C4DA
 1.5 with sigma of 0.02
 C7BA-C6B
 1.5 with sigma of 0.02
 C7BB-C6B
 1.5 with sigma of 0.02
 C7DA-C6D
 1.3 with sigma of 0.02
 N2C-C6CA
 1.45 with sigma of 0.02
 C6CA-C7CA
 1.45 with sigma of 0.02
 C7DA-C7DB
 1.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C4DA \\sim C5DA \\sim C4DB \\sim C5DB: within 2A with sigma of 0.001 and sigma
for terminal atoms of 0.002
C7BA \\sim C7BB: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
C6D \\sim C7DA: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
Uanis(C7CA) \\sim Ueq, Uanis(C7DA) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C6CA) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Others
 Sof(C4DB)=Sof(H4DC)=Sof(H4DD)=Sof(C5DB)=Sof(H5DD)=Sof(H5DE)=Sof(H5DF)=1-FVAR(1)
 Sof(C4DA)=Sof(H4DA)=Sof(H4DB)=Sof(C5DA)=Sof(H5DA)=Sof(H5DB)=Sof(H5DC)=FVAR(1)
 Sof(H6BC)=Sof(H6BD)=Sof(C7BB)=Sof(H7BA)=Sof(H7BB)=1-FVAR(2)
 Sof(H6BA)=Sof(H6BB)=Sof(C7BA)=Sof(H7BC)=Sof(H7BD)=FVAR(2)
 Fixed Sof: C6CA(0.5) C7CA(0.5) C7DA(0.5) C7DB(0.5) C7CB(0.5) C6CB(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C4A(H4AA,H4AB), C6A(H6AA,H6AB), C7A(H7AA,H7AB), C4B(H4BA,H4BB), C6B(H6BC,
 H6BD), C6B(H6BA,H6BB), C7BB(H7BA,H7BB), C7BA(H7BC,H7BD), C4DA(H4DA,H4DB),
 C4DB(H4DC,H4DD)
5.b Aromatic/amide H refined with riding coordinates:
 C1A(H1A), C2A(H2A), C1B(H1B), C2B(H2B), C1C(H1C), C2C(H2C), C4C(H4C),
 C1D(H1D), C2D(H2D)
5.c Idealised Me refined as rotating group:
 C5A(H5AA,H5AB,H5AC), C5B(H5BA,H5BB,H5BC), C5C(H5CA,H5CB,H5CC), C5DA(H5DA,H5DB,
 H5DC), C5DB(H5DD,H5DE,H5DF)
;