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_7117074
_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_absolute_configuration unk
_chemical_formula_moiety         'Cu3 I6, 1.5(C14 H30 N2)'
_chemical_formula_sum            'C21 H45 Cu3 I6 N3'
_chemical_formula_weight         1291.62
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_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                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.52016(18)
_cell_length_b                   31.2866(8)
_cell_length_c                   13.2813(3)
_cell_measurement_temperature    99.8(2)
_cell_volume                     3540.35(14)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      99.8(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0327
_diffrn_reflns_av_unetI/netI     0.0320
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            24663
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.72
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    7.033
_exptl_absorpt_correction_T_max  0.7200
_exptl_absorpt_correction_T_min  0.1562
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.423
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       column
_exptl_crystal_F_000             2388
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.579
_refine_diff_density_min         -2.380
_refine_diff_density_rms         0.156
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.50(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         6233
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.0320
_refine_ls_R_factor_gt           0.0299
_refine_ls_shift/su_max          0.175
_refine_ls_shift/su_mean         0.011
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0111P)^2^+23.7137P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0600
_refine_ls_wR_factor_ref         0.0611
_reflns_number_gt                6005
_reflns_number_total             6233
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5cc01154j2.cif
_cod_data_source_block           100K
_cod_original_cell_volume        3540.36(14)
_cod_database_code               7117074
_olex2_refinement_description
;
1. Others
 Fixed Sof: N3(0.5) C19(0.5) H19A(0.5) H19B(0.5) C22(0.5) H22A(0.5) H22B(0.5)
 C21(0.5) H21A(0.5) H21B(0.5) C20(0.5) H20A(0.5) H20B(0.5) C23(0.5) H23A(0.5)
 H23B(0.5) C24(0.5) H24A(0.5) H24B(0.5) N4(0.5)
 Fixed Uiso: H1A(0.067) H1B(0.067) H1C(0.067) H2A(0.034) H2B(0.034) H3A(0.029)
 H3B(0.029) H4A(0.024) H4B(0.024) H5A(0.025) H5B(0.025) H6A(0.019) H6B(0.019)
 H7A(0.026) H7B(0.026) H8A(0.023) H8B(0.023) H9A(0.029) H9B(0.029) H10A(0.023)
 H10B(0.023) H11A(0.026) H11B(0.026) H12A(0.03) H12B(0.03) H13A(0.032)
 H13B(0.032) H14A(0.056) H14B(0.056) H14C(0.056) H15A(0.097) H15B(0.097)
 H15C(0.097) H16A(0.048) H16B(0.048) H17A(0.041) H17B(0.041) H18A(0.047)
 H18B(0.047) H19A(0.029) H19B(0.029) H22A(0.036) H22B(0.036) H21A(0.036)
 H21B(0.036) H20A(0.039) H20B(0.039) H23A(0.022) H23B(0.022) H24A(0.022)
 H24B(0.022)
 Fixed X: H1A(0.8635) H1B(0.8267) H1C(0.7312) H2A(0.6242) H2B(0.5771)
 H3A(0.8303) H3B(0.7626) H4A(0.6022) H4B(0.5239) H5A(0.5626) H5B(0.723)
 H6A(0.8573) H6B(0.6946) H7A(0.918) H7B(0.8558) H8A(0.8606) H8B(0.9803)
 H9A(0.5875) H9B(0.4605) H10A(0.5189) H10B(0.5939) H11A(0.8514) H11B(0.9)
 H12A(0.6022) H12B(0.6474) H13A(0.808) H13B(0.8341) H14A(0.5573) H14B(0.5777)
 H14C(0.6791) H15A(0.1059) H15B(0.2028) H15C(0.2824) H16A(0.3609) H16B(0.1856)
 H17A(0.3231) H17B(0.1514) H18A(0.4255) H18B(0.2571) H19A(0.2325) H19B(0.4162)
 H22A(0.4141) H22B(0.5355) H21A(0.4774) H21B(0.5553) H20A(0.4387) H20B(0.2571)
 H23A(0.17) H23B(0.0802) H24A(0.0718) H24B(0.1289)
 Fixed Y: H1A(0.8918) H1B(0.9046) H1C(0.9252) H2A(0.8583) H2B(0.8735)
 H3A(0.8166) H3B(0.8287) H4A(0.781) H4B(0.7957) H5A(0.7512) H5B(0.7761)
 H6A(0.7194) H6B(0.7024) H7A(0.7523) H7B(0.7361) H8A(0.6683) H8B(0.6844)
 H9A(0.7023) H9B(0.7188) H10A(0.6697) H10B(0.6453) H11A(0.6148) H11B(0.6412)
 H12A(0.6038) H12B(0.6313) H13A(0.5545) H13B(0.5807) H14A(0.5356) H14B(0.5632)
 H14C(0.5219) H15A(0.5562) H15B(0.5946) H15C(0.5498) H16A(0.594) H16B(0.6035)
 H17A(0.5214) H17B(0.533) H18A(0.5679) H18B(0.5834) H19A(0.4721) H19B(0.4759)
 H22A(0.5224) H22B(0.4883) H21A(0.5595) H21B(0.5199) H20A(0.4358) H20B(0.4271)
 H23A(0.5589) H23B(0.5287) H24A(0.4765) H24B(0.5103)
 Fixed Z: H1A(0.6809) H1B(0.7926) H1C(0.7041) H2A(0.667) H2B(0.7754)
 H3A(0.7418) H3B(0.8479) H4A(0.7013) H4B(0.8021) H5A(0.9572) H5B(0.956)
 H6A(1.0021) H6B(1.0408) H7A(0.8247) H7B(0.72) H8A(0.7674) H8B(0.8491)
 H9A(0.7222) H9B(0.7986) H10A(0.9107) H10B(0.8189) H11A(0.9074) H11B(1.0026)
 H12A(0.9753) H12B(1.0699) H13A(1.02) H13B(1.1193) H14A(1.0729) H14B(1.1706)
 H14C(1.1553) H15A(0.9365) H15B(0.9798) H15C(0.9662) H16A(0.8357) H16B(0.8082)
 H17A(0.7849) H17B(0.7515) H18A(0.6678) H18B(0.6383) H19A(0.6487) H19B(0.6516)
 H22A(0.3491) H22B(0.389) H21A(0.4828) H21B(0.5352) H20A(0.5169) H20B(0.5229)
 H23A(0.4851) H23B(0.5597) H24A(0.4477) H24B(0.3676)
;