#------------------------------------------------------------------------------
#$Date: 2017-11-07 02:27:57 +0200 (Tue, 07 Nov 2017) $
#$Revision: 202662 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/00/28/4002860.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4002860
loop_
_publ_author_name
'Yu, Muxin'
'Chen, Lian'
'Jiang, Feilong'
'Zhou, Kang'
'Liu, Caiping'
'Sun, Cai'
'Li, Xingjun'
'Yang, Yan'
'Hong, Maochun'
_publ_section_title
;
 Cation-Induced Strategy toward an Hourglass-Shaped Cu6I7-- Cluster and
 Its Color-Tunable Luminescence
;
_journal_issue                   19
_journal_name_full               'Chemistry of Materials'
_journal_page_first              8093
_journal_paper_doi               10.1021/acs.chemmater.7b01790
_journal_volume                  29
_journal_year                    2017
_chemical_formula_sum            'C15 H15 Cu I N6 O P'
_chemical_formula_weight         516.74
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/4
_cell_angle_alpha                116.350(6)
_cell_angle_beta                 102.549(6)
_cell_angle_gamma                96.607(5)
_cell_formula_units_Z            2
_cell_length_a                   9.0437(6)
_cell_length_b                   10.8072(6)
_cell_length_c                   10.8381(7)
_cell_measurement_reflns_used    5095
_cell_measurement_temperature    100.00(11)
_cell_measurement_theta_max      72.9520
_cell_measurement_theta_min      4.6790
_cell_volume                     899.05(12)
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.00(11)
_diffrn_detector_area_resol_mean 10.5594
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'SuperNova (Cu) X-ray Source'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0360
_diffrn_reflns_av_unetI/netI     0.0424
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8514
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.141
_diffrn_reflns_theta_min         4.706
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    16.184
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56280
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.909
_exptl_crystal_description       block
_exptl_crystal_F_000             504
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.689
_refine_diff_density_min         -0.755
_refine_diff_density_rms         0.149
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         3506
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0345
_refine_ls_R_factor_gt           0.0315
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0504P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0793
_refine_ls_wR_factor_ref         0.0819
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3279
_reflns_number_total             3506
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            cm7b01790_si_003.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 4002860--4002865.cif.'
_cod_original_cell_volume        899.05(11)
_cod_database_code               4002860
_shelx_shelxl_version_number     2016/4
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
I1 I 0.04924(2) 0.22221(2) 0.02566(2) 0.01829(9) Uani 1 1 d . .
CU1 Cu -0.03031(6) 0.05191(6) 0.12457(6) 0.01843(13) Uani 1 1 d . .
P1 P 0.43369(10) 0.55024(10) 0.81658(9) 0.01665(19) Uani 1 1 d . .
O1 O 0.3563(3) 0.5633(3) 0.9271(3) 0.0225(6) Uani 1 1 d . .
N1 N 0.1212(3) 0.1218(4) 0.3270(3) 0.0197(6) Uani 1 1 d . .
N2 N 0.3144(3) 0.4653(4) 0.6485(3) 0.0182(6) Uani 1 1 d . .
H2 H 0.287247 0.517738 0.608371 0.022 Uiso 1 1 calc R U
N5 N 0.5196(3) 0.7001(4) 0.8285(3) 0.0191(6) Uani 1 1 d . .
H5 H 0.620275 0.712295 0.838593 0.023 Uiso 1 1 calc R U
N3 N 0.5736(3) 0.4674(4) 0.8273(3) 0.0193(6) Uani 1 1 d . .
H3 H 0.589639 0.446695 0.898250 0.023 Uiso 1 1 calc R U
N6 N 0.2435(3) 0.9270(4) 0.8391(3) 0.0189(6) Uani 1 1 d . .
N4 N 0.7441(4) 0.3989(4) 0.5296(4) 0.0216(7) Uani 1 1 d . .
C12 C 0.6707(4) 0.4251(4) 0.7390(4) 0.0186(7) Uani 1 1 d . .
C18 C 0.4550(4) 0.8104(4) 0.8249(4) 0.0181(7) Uani 1 1 d . .
C11 C 0.1354(5) 0.0319(5) 0.3813(5) 0.0261(8) Uani 1 1 d . .
H11 H 0.097212 -0.067596 0.317900 0.031 Uiso 1 1 calc R U
C8 C 0.2531(4) 0.3186(4) 0.5650(4) 0.0187(7) Uani 1 1 d . .
C17 C 0.3047(4) 0.8190(4) 0.8374(4) 0.0181(7) Uani 1 1 d . .
H17 H 0.244457 0.746125 0.844951 0.022 Uiso 1 1 calc R U
C16 C 0.8671(5) 0.3531(5) 0.5713(5) 0.0277(9) Uani 1 1 d . .
H16 H 0.935403 0.327946 0.513575 0.033 Uiso 1 1 calc R U
C7 C 0.1809(4) 0.2612(4) 0.4172(4) 0.0180(7) Uani 1 1 d . .
H7 H 0.173623 0.324543 0.378497 0.022 Uiso 1 1 calc R U
C15 C 0.8978(5) 0.3411(5) 0.6964(5) 0.0275(9) Uani 1 1 d . .
H15 H 0.986191 0.308513 0.723261 0.033 Uiso 1 1 calc R U
C19 C 0.5418(4) 0.9171(4) 0.8122(4) 0.0202(7) Uani 1 1 d . .
H19 H 0.643737 0.914377 0.803375 0.024 Uiso 1 1 calc R U
C9 C 0.2617(5) 0.2243(5) 0.6203(4) 0.0242(8) Uani 1 1 d . .
H9 H 0.306667 0.258546 0.720693 0.029 Uiso 1 1 calc R U
C14 C 0.7991(4) 0.3770(5) 0.7820(4) 0.0221(8) Uani 1 1 d . .
H14 H 0.818299 0.368989 0.867601 0.026 Uiso 1 1 calc R U
C13 C 0.6490(4) 0.4338(4) 0.6120(4) 0.0199(7) Uani 1 1 d . .
H13 H 0.561846 0.466343 0.582395 0.024 Uiso 1 1 calc R U
C20 C 0.4768(4) 1.0268(5) 0.8126(4) 0.0222(8) Uani 1 1 d . .
H20 H 0.533292 1.100357 0.803314 0.027 Uiso 1 1 calc R U
C10 C 0.2037(6) 0.0799(5) 0.5264(5) 0.0328(9) Uani 1 1 d . .
H10 H 0.210970 0.013951 0.561846 0.039 Uiso 1 1 calc R U
C21 C 0.3275(4) 1.0282(5) 0.8268(4) 0.0210(7) Uani 1 1 d . .
H21 H 0.283912 1.104435 0.827787 0.025 Uiso 1 1 calc R U
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.3257 6.8362 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
CU1 I1 CU1 60.28(2) . 2
N1 CU1 N6 103.91(12) . 2_566
N1 CU1 I1 109.37(10) . .
N6 CU1 I1 108.60(9) 2_566 .
N1 CU1 I1 106.76(9) . 2
N6 CU1 I1 107.35(10) 2_566 2
I1 CU1 I1 119.72(2) . 2
N1 CU1 CU1 128.11(8) . 2
N6 CU1 CU1 127.92(9) 2_566 2
I1 CU1 CU1 60.22(2) . 2
I1 CU1 CU1 59.50(2) 2 2
O1 P1 N3 109.46(15) . .
O1 P1 N5 116.65(17) . .
N3 P1 N5 104.83(16) . .
O1 P1 N2 114.23(16) . .
N3 P1 N2 108.82(16) . .
N5 P1 N2 102.16(16) . .
C7 N1 C11 118.1(3) . .
C7 N1 CU1 120.4(2) . .
C11 N1 CU1 120.0(3) . .
C8 N2 P1 126.0(3) . .
C8 N2 H2 117.0 . .
P1 N2 H2 117.0 . .
C18 N5 P1 129.1(3) . .
C18 N5 H5 115.4 . .
P1 N5 H5 115.4 . .
C12 N3 P1 129.0(3) . .
C12 N3 H3 115.5 . .
P1 N3 H3 115.5 . .
C21 N6 C17 118.8(3) . .
C21 N6 CU1 119.2(2) . 2_566
C17 N6 CU1 121.8(3) . 2_566
C13 N4 C16 118.3(3) . .
C13 C12 C14 117.9(3) . .
C13 C12 N3 123.0(3) . .
C14 C12 N3 119.1(3) . .
C19 C18 N5 120.0(3) . .
C19 C18 C17 118.5(3) . .
N5 C18 C17 121.5(3) . .
N1 C11 C10 121.9(4) . .
N1 C11 H11 119.0 . .
C10 C11 H11 119.0 . .
C9 C8 N2 123.7(3) . .
C9 C8 C7 117.4(4) . .
N2 C8 C7 118.8(3) . .
N6 C17 C18 122.1(4) . .
N6 C17 H17 118.9 . .
C18 C17 H17 118.9 . .
N4 C16 C15 122.0(3) . .
N4 C16 H16 119.0 . .
C15 C16 H16 119.0 . .
N1 C7 C8 123.6(3) . .
N1 C7 H7 118.2 . .
C8 C7 H7 118.2 . .
C14 C15 C16 119.9(3) . .
C14 C15 H15 120.1 . .
C16 C15 H15 120.1 . .
C20 C19 C18 118.8(3) . .
C20 C19 H19 120.6 . .
C18 C19 H19 120.6 . .
C10 C9 C8 118.9(4) . .
C10 C9 H9 120.5 . .
C8 C9 H9 120.5 . .
C15 C14 C12 118.3(3) . .
C15 C14 H14 120.9 . .
C12 C14 H14 120.9 . .
N4 C13 C12 123.7(3) . .
N4 C13 H13 118.2 . .
C12 C13 H13 118.2 . .
C19 C20 C21 119.2(4) . .
C19 C20 H20 120.4 . .
C21 C20 H20 120.4 . .
C11 C10 C9 119.9(4) . .
C11 C10 H10 120.0 . .
C9 C10 H10 120.0 . .
N6 C21 C20 122.6(4) . .
N6 C21 H21 118.7 . .
C20 C21 H21 118.7 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
I1 CU1 2.6145(6) .
I1 CU1 2.6338(6) 2
CU1 N1 2.061(3) .
CU1 N6 2.068(3) 2_566
CU1 I1 2.6338(6) 2
CU1 CU1 2.6355(10) 2
P1 O1 1.478(3) .
P1 N3 1.644(3) .
P1 N5 1.650(4) .
P1 N2 1.661(3) .
N1 C7 1.339(5) .
N1 C11 1.346(5) .
N2 C8 1.395(5) .
N2 H2 0.8800 .
N5 C18 1.399(5) .
N5 H5 0.8800 .
N3 C12 1.402(4) .
N3 H3 0.8800 .
N6 C21 1.332(5) .
N6 C17 1.342(5) .
N6 CU1 2.068(3) 2_566
N4 C13 1.337(5) .
N4 C16 1.340(5) .
C12 C13 1.394(5) .
C12 C14 1.398(5) .
C18 C19 1.394(6) .
C18 C17 1.404(5) .
C11 C10 1.380(6) .
C11 H11 0.9500 .
C8 C9 1.394(5) .
C8 C7 1.395(5) .
C17 H17 0.9500 .
C16 C15 1.390(6) .
C16 H16 0.9500 .
C7 H7 0.9500 .
C15 C14 1.389(5) .
C15 H15 0.9500 .
C19 C20 1.381(5) .
C19 H19 0.9500 .
C9 C10 1.384(7) .
C9 H9 0.9500 .
C14 H14 0.9500 .
C13 H13 0.9500 .
C20 C21 1.393(5) .
C20 H20 0.9500 .
C10 H10 0.9500 .
C21 H21 0.9500 .
