An organic-ligand-free thermochromic luminescent cuprous iodide trinuclear cluster: evidence for cluster centered emission and configuration distortion with temperature
Shi-Li Li; Fu-Qiang Zhang; Xian-Ming Zhang; Chem.Commun. 51 (2015) 8062–; doi:10.1039/C5cc01154J

data_7117076
_publ_section_title
;
 An organic-ligand-free thermochromic luminescent cuprous iodide
 trinuclear cluster: evidence for cluster centered emission and
 configuration distortion with temperature
;
_journal_name_full               Chem.Commun.
_journal_page_first              8062
_journal_paper_doi               10.1039/C5cc01154J
_journal_volume                  51
_journal_year                    2015
_chemical_formula_moiety         'Cu3.01 I6, 1.5(C14 H30 N2)'
_chemical_formula_sum            'C21 H45 Cu3.01 I6 N3'
_chemical_formula_weight         1292.28
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2bc 2'
_space_group_name_H-M_alt        'P 2 21 21'
_symmetry_space_group_name_Hall  'P 2bc 2'
_symmetry_space_group_name_H-M   'P 2 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2014-11-23
_audit_creation_method
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_audit_update_record
;
2015-01-29 deposited with the CCDC.
2015-03-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.5719(8)
_cell_length_b                   13.4018(7)
_cell_length_c                   31.305(3)
_cell_measurement_reflns_used    1744
_cell_measurement_temperature    200.2(3)
_cell_measurement_theta_max      27.5090
_cell_measurement_theta_min      3.8910
_cell_volume                     3596.3(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      200.2(3)
_diffrn_detector_area_resol_mean 16.0710
_diffrn_measured_fraction_theta_full 0.628
_diffrn_measured_fraction_theta_max 0.700
_diffrn_measurement_details
;
  1 omega  -36.00   41.00   1.0000   26.0000
omega____ theta____ kappa____ phi______ frames
    -       18.1748  -19.0000 -120.0000 77
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0014188000
_diffrn_orient_matrix_UB_12      -0.0442453000
_diffrn_orient_matrix_UB_13      0.0123849000
_diffrn_orient_matrix_UB_21      0.0006163000
_diffrn_orient_matrix_UB_22      0.0290231000
_diffrn_orient_matrix_UB_23      0.0189478000
_diffrn_orient_matrix_UB_31      -0.0828123000
_diffrn_orient_matrix_UB_32      -0.0005408000
_diffrn_orient_matrix_UB_33      0.0003698000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0181
_diffrn_reflns_av_unetI/netI     0.0439
_diffrn_reflns_Laue_measured_fraction_full 0.628
_diffrn_reflns_Laue_measured_fraction_max 0.700
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            4824
_diffrn_reflns_point_group_measured_fraction_full 0.555
_diffrn_reflns_point_group_measured_fraction_max 0.621
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         24.995
_diffrn_reflns_theta_min         2.895
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.930
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89504
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.387
_exptl_crystal_description       column
_exptl_crystal_F_000             2389
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.609
_refine_diff_density_min         -0.709
_refine_diff_density_rms         0.100
_refine_ls_abs_structure_details
;
 Flack x determined using 1189 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.45(3)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     333
_refine_ls_number_reflns         3932
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_gt           0.0295
_refine_ls_shift/su_max          0.085
_refine_ls_shift/su_mean         0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0129P)^2^+4.8421P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0543
_refine_ls_wR_factor_ref         0.0570
_reflns_Friedel_coverage         0.563
_reflns_Friedel_fraction_full    0.460
_reflns_Friedel_fraction_max     0.518
_reflns_number_gt                3521
_reflns_number_total             3932
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc01154j2.cif
_cod_data_source_block           200k
_cod_database_code               7117076
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         'C N H Cu I'
_shelx_estimated_absorpt_t_max   0.723
_shelx_estimated_absorpt_t_min   0.159
_reflns_odcompleteness_completeness 68.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C21) = Uanis(C22)
Uanis(C23) = Uanis(C24)
3. Others
 Fixed Sof: N3(0.5) C21(0.5) H21A(0.5) H21B(0.5) C23(0.5) H23A(0.5) H23B(0.5)
 C19(0.5) H19A(0.5) H19B(0.5) C22(0.5) H22A(0.5) H22B(0.5) C24(0.5) H24A(0.5)
 H24B(0.5) C20(0.5) H20A(0.5) H20B(0.5) N4(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B),
 C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B),
 C13(H13A,H13B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C21(H21A,H21B),
  C23(H23A,H23B), C19(H19A,H19B), C22(H22A,H22B), C24(H24A,H24B), C20(H20A,H20B)
4.b Me refined with riding coordinates:
 C1(H1A,H1B,H1C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C)
;