#------------------------------------------------------------------------------
#$Date: 2019-03-22 01:14:15 +0200 (Fri, 22 Mar 2019) $
#$Revision: 214275 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/31/7123173.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_7123173
loop_
_publ_author_name
'Li, Dan'
'Yang, Hu'
'Zheng, Ji'
'Peng, Su-Kao'
'Zhu, Xiao-Wei'
'Wan, Meng-Yan'
'Lu, Weigang'
_publ_section_title
;
 A Chemopalette Strategy for White Light by Modulating Monomeric and
 Excimeric Phosphorescence of a Simple Cu(I) Cyclic Trinuclear Unit
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC00716D
_journal_year                    2019
_chemical_formula_moiety         'C9 H6 Cl3 Cu3 N6'
_chemical_formula_sum            'C9 H6 Cl3 Cu3 N6'
_chemical_formula_weight         495.17
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2019-02-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-02-16 deposited with the CCDC.    2019-03-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.3157(4)
_cell_length_b                   11.6083(3)
_cell_length_c                   7.6970(2)
_cell_measurement_reflns_used    2076
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      76.2360
_cell_measurement_theta_min      4.6440
_cell_volume                     1457.79(6)
_computing_cell_refinement       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.930
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -74.00 -31.00   0.50    6.21    --   -0.90 -26.00  13.00   86
  2  ω      6.00  31.00   0.50    6.21    --   -0.90  26.00 176.00   50
  3  ω     72.00  99.00   0.50   24.85    --  105.10 -26.00  13.00   54
  4  ω    112.00 137.00   0.50   24.85    --  105.10  26.00 176.00   50
  5  ω    -32.00  16.00   0.50    6.21    --   -0.90  82.00-180.00   96
  6  ω    -32.00  34.00   0.50    6.21    --    0.90  82.00  90.00  132
  7  ω     18.00 132.00   0.50   24.85    --  105.10 -57.00   0.00  228
  8  ω     51.00 138.00   0.50   24.85    --  105.10 -77.00 -90.00  174
  9  ω    126.00 151.00   0.50   24.85    --  105.10  82.00-150.00   50
 10  ω     73.00 124.00   0.50   24.85    --  105.10 -38.00 150.00  102
 11  ω    162.00 187.00   0.50   24.85    --  105.10  82.00  30.00   50
 12  ω    107.00 132.00   0.50   24.85    --  105.10  82.00  30.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0395978000
_diffrn_orient_matrix_UB_12      -0.1204121000
_diffrn_orient_matrix_UB_13      0.0053951000
_diffrn_orient_matrix_UB_21      0.0801634000
_diffrn_orient_matrix_UB_22      -0.0535469000
_diffrn_orient_matrix_UB_23      -0.0681488000
_diffrn_orient_matrix_UB_31      0.0301983000
_diffrn_orient_matrix_UB_32      -0.0157683000
_diffrn_orient_matrix_UB_33      0.1882148000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0557
_diffrn_reflns_av_unetI/netI     0.0531
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.930
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            4789
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.930
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.328
_diffrn_reflns_theta_min         4.675
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    10.147
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.52819
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.33c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.256
_exptl_crystal_description       needle
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.636
_refine_diff_density_min         -0.544
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     97
_refine_ls_number_reflns         1444
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0787
_refine_ls_R_factor_gt           0.0538
_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)+(0.0964P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1316
_refine_ls_wR_factor_ref         0.1428
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1096
_reflns_number_total             1444
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9cc00716d2.cif
_cod_data_source_block           cl-alpha-150k
_cod_original_cell_volume        1457.78(7)
_cod_database_code               7123173
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'Cu Cl C H N'
_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.
;
_shelx_estimated_absorpt_t_max   0.402
_shelx_estimated_absorpt_t_min   0.236
_reflns_odcompleteness_completeness 99.28
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5)
;
_shelx_res_file
;
TITL Cl-alpha-150K in Pbcn #60
    cl-alpha-150k.res
    created by SHELXL-2016/6 at 21:53:35 on 15-Feb-2019
REM reset to Pbcn #60
CELL 1.54184 16.315681 11.60825 7.696953 90 90 90
ZERR 4 0.000414 0.000299 0.00023 0 0 0
LATT 1
SYMM 0.5-X,0.5-Y,0.5+Z
SYMM 0.5+X,0.5-Y,-Z
SYMM -X,+Y,0.5-Z
SFAC C H N Cl Cu
UNIT 36 24 24 12 12

L.S. 10 0 0
PLAN  1
SIZE 0.2 0.15 0.11
TEMP -123.15(10)
BOND
fmap 2 53
acta
OMIT 1 5 9
OMIT 1 2 9
OMIT 1 1 9
OMIT 5 8 5
OMIT 0 2 9
OMIT 5 7 8
OMIT 0 8 0
OMIT 3 4 9
OMIT 2 4 9
OMIT 0 6 8
OMIT 0 4 9
OMIT 4 4 9
OMIT 2 1 9
OMIT 2 2 9
OMIT 3 10 7
OMIT 3 2 9
OMIT 3 8 8
OMIT 4 1 9
OMIT 7 1 0
OMIT 9 5 8
OMIT 1 1 5
OMIT 1 4 6
OMIT 1 7 5
OMIT 1 11 6
OMIT 6 7 4
OMIT 7 1 8
OMIT 5 11 1
OMIT 0 0 8
OMIT 1 0 8
OMIT 11 12 2
OMIT 0 8 2
OMIT 8 6 8
OMIT 0 2 8
OMIT 1 8 4
OMIT 13 3 7
OMIT 1 1 8
OMIT 9 10 3
OMIT 4 0 0
OMIT 10 2 8
OMIT 3 2 8
OMIT 6 7 6
OMIT 1 7 6
OMIT 0 8 8
OMIT 6 3 1
OMIT 10 0 2
OMIT 7 2 9
OMIT 18 0 4
OMIT 14 1 6
OMIT 3 1 9
OMIT 12 2 7
REM <olex2.extras>
REM <HklSrc "%.\\Cl-alpha-150K.hkl">
REM </olex2.extras>

WGHT    0.096400
FVAR       0.80621
CU1   5    0.415774    0.821967    0.135483    11.00000    0.04834    0.02833 =
         0.04422    0.00120   -0.00292    0.00453
CU2   5    0.500000    1.063496    0.250000    10.50000    0.03760    0.03716 =
         0.04193    0.00000   -0.00326    0.00000
CL1   4    0.500000    0.354138    0.250000    10.50000    0.04572    0.02689 =
         0.05190    0.00000    0.00135    0.00000
CL2   4    0.216897    1.178399   -0.139314    11.00000    0.04722    0.04057 =
         0.05641    0.00146   -0.01015    0.01079
N1    3    0.462835    0.683495    0.207019    11.00000    0.04537    0.03125 =
         0.03851    0.00268   -0.00320   -0.00013
N2    3    0.370436    0.961378    0.065250    11.00000    0.04193    0.03162 =
         0.03587    0.00164    0.00222    0.00290
N3    3    0.408679    1.062590    0.105658    11.00000    0.03733    0.03639 =
         0.03723    0.00241   -0.00276    0.00023
C1    1    0.500000    0.502164    0.250000    10.50000    0.04169    0.02406 =
         0.03462    0.00000    0.00100    0.00000
C2    1    0.440166    0.574464    0.181494    11.00000    0.04315    0.02942 =
         0.04589   -0.00337   -0.00441   -0.00063
AFIX  43
H2    2    0.391199    0.550136    0.125693    11.00000   -1.20000
AFIX   0
C3    1    0.300339    0.985876   -0.019546    11.00000    0.03986    0.03091 =
         0.03839    0.00285    0.00056   -0.00209
AFIX  43
H3    2    0.261834    0.931153   -0.061503    11.00000   -1.20000
AFIX   0
C4    1    0.293955    1.104259   -0.035144    11.00000    0.04109    0.03078 =
         0.03535   -0.00020    0.00024    0.00467
C5    1    0.362598    1.148967    0.043836    11.00000    0.04135    0.03015 =
         0.03709    0.00101    0.00067    0.00197
AFIX  43
H5    2    0.375341    1.228584    0.053105    11.00000   -1.20000
AFIX   0
HKLF 4




REM  Cl-alpha-150K in Pbcn #60
REM R1 =  0.0538 for    1096 Fo > 4sig(Fo)  and  0.0787 for all    1444 data
REM     97 parameters refined using      0 restraints

END

WGHT      0.0964      0.0000

REM Highest difference peak  0.636,  deepest hole -0.544,  1-sigma level  0.139
Q1    1   0.4461  1.0335  0.1661  11.00000  0.05    0.64
;
_shelx_res_checksum              5392
_olex2_submission_original_sample_id Cl-alpha-150K
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.757
_oxdiff_exptl_absorpt_empirical_full_min 0.386
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y, z-1/2'
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
_atom_site_refinement_flags_occupancy
Cu1 Cu 0.41577(5) 0.82197(6) 0.13548(10) 0.0403(3) Uani 1 1 d . . .
Cu2 Cu 0.500000 1.06350(8) 0.250000 0.0389(3) Uani 1 2 d S T P
Cl1 Cl 0.500000 0.35414(13) 0.250000 0.0415(4) Uani 1 2 d S T P
Cl2 Cl 0.21690(8) 1.17840(10) -0.13931(19) 0.0481(4) Uani 1 1 d . . .
N1 N 0.4628(3) 0.6835(3) 0.2070(6) 0.0384(9) Uani 1 1 d . . .
N2 N 0.3704(2) 0.9614(3) 0.0652(6) 0.0365(9) Uani 1 1 d . . .
N3 N 0.4087(2) 1.0626(3) 0.1057(6) 0.0370(9) Uani 1 1 d . . .
C1 C 0.500000 0.5022(5) 0.250000 0.0335(13) Uani 1 2 d S T P
C2 C 0.4402(3) 0.5745(4) 0.1815(7) 0.0395(11) Uani 1 1 d . . .
H2 H 0.391199 0.550136 0.125693 0.047 Uiso 1 1 calc R . .
C3 C 0.3003(3) 0.9859(4) -0.0195(7) 0.0364(10) Uani 1 1 d . . .
H3 H 0.261834 0.931153 -0.061503 0.044 Uiso 1 1 calc R . .
C4 C 0.2940(3) 1.1043(4) -0.0351(6) 0.0357(10) Uani 1 1 d . . .
C5 C 0.3626(3) 1.1490(4) 0.0438(6) 0.0362(10) Uani 1 1 d . . .
H5 H 0.375341 1.228584 0.053105 0.043 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu1 0.0483(5) 0.0283(4) 0.0442(5) 0.0012(3) -0.0029(3) 0.0045(3)
Cu2 0.0376(5) 0.0372(6) 0.0419(7) 0.000 -0.0033(4) 0.000
Cl1 0.0457(8) 0.0269(7) 0.0519(10) 0.000 0.0013(7) 0.000
Cl2 0.0472(7) 0.0406(6) 0.0564(9) 0.0015(5) -0.0102(6) 0.0108(5)
N1 0.045(2) 0.0313(19) 0.039(2) 0.0027(16) -0.0032(18) -0.0001(16)
N2 0.042(2) 0.0316(18) 0.036(2) 0.0016(16) 0.0022(17) 0.0029(15)
N3 0.037(2) 0.036(2) 0.037(2) 0.0024(17) -0.0028(17) 0.0002(14)
C1 0.042(3) 0.024(3) 0.035(4) 0.000 0.001(3) 0.000
C2 0.043(3) 0.029(2) 0.046(3) -0.0034(19) -0.004(2) -0.0006(17)
C3 0.040(2) 0.031(2) 0.038(3) 0.0028(19) 0.0006(19) -0.0021(17)
C4 0.041(2) 0.0308(19) 0.035(3) 0.000(2) 0.0002(19) 0.0047(18)
C5 0.041(2) 0.030(2) 0.037(3) 0.001(2) 0.0007(19) 0.0020(17)
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'
Cl Cl 0.3639 0.7018 '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'
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
N2 Cu1 N1 179.03(19) . .
N3 Cu2 N3 179.4(3) . 4_655
N1 N1 Cu1 120.20(13) 4_655 .
C2 N1 Cu1 131.4(4) . .
C2 N1 N1 108.3(3) . 4_655
N3 N2 Cu1 120.0(3) . .
C3 N2 Cu1 131.5(3) . .
C3 N2 N3 108.5(4) . .
N2 N3 Cu2 120.5(3) . .
C5 N3 Cu2 131.1(3) . .
C5 N3 N2 107.8(4) . .
C2 C1 Cl1 127.1(3) . .
C2 C1 Cl1 127.1(3) 4_655 .
C2 C1 C2 105.8(6) . 4_655
N1 C2 C1 108.8(4) . .
N2 C3 C4 108.4(4) . .
C3 C4 Cl2 126.3(4) . .
C5 C4 Cl2 127.7(4) . .
C5 C4 C3 106.0(4) . .
N3 C5 C4 109.3(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 N1 1.865(4) .
Cu1 N2 1.860(4) .
Cu2 N3 1.859(4) 4_655
Cu2 N3 1.859(4) .
Cl1 C1 1.718(6) .
Cl2 C4 1.722(5) .
N1 N1 1.382(8) 4_655
N1 C2 1.333(6) .
N2 N3 1.366(5) .
N2 C3 1.347(6) .
N3 C5 1.341(6) .
C1 C2 1.391(6) .
C1 C2 1.391(6) 4_655
C3 C4 1.383(6) .
C4 C5 1.376(6) .
