#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:43:37 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179344 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/41/4324126.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_4324126
loop_
_publ_author_name
'Lei Hou'
'Wen-Juan Shi'
'Yao-Yu Wang'
'Hai-Hua Wang'
'Lin Cui'
'Peng-Xiang Chen'
'Qi-Zhen Shi'
_publ_section_title
;
 Trinuclear-based Copper(I) Pyrazolate Polymers: Effect of Trimer
 π-Acid...Halide/Pseudohalide Interactions on the Supramolecular
 Structure and Phosphorescence
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              261
_journal_page_last               270
_journal_paper_doi               10.1021/ic101901w
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C36 H42 Cl Cu4 N9'
_chemical_formula_weight         890.40
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 100.719(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.571(2)
_cell_length_b                   19.468(5)
_cell_length_c                   12.930(4)
_cell_measurement_reflns_used    1040
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      23.78
_cell_measurement_theta_min      2.73
_cell_volume                     1872.5(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0628
_diffrn_reflns_av_sigmaI/netI    0.0830
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            10235
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         1.91
_exptl_absorpt_coefficient_mu    2.351
_exptl_absorpt_correction_T_max  0.7989
_exptl_absorpt_correction_T_min  0.6769
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.579
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       sheet
_exptl_crystal_F_000             908
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.741
_refine_diff_density_min         -0.624
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         3793
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.1255
_refine_ls_R_factor_gt           0.0624
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0885P)²+1.6442P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1587
_refine_ls_wR_factor_ref         0.1974
_reflns_number_gt                1977
_reflns_number_total             3793
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic101901w_si_002_1.cif
_cod_data_source_block           complex_1
_cod_original_cell_volume        1872.6(9)
_cod_database_code               4324126
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, 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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl2 Cl 1.3519(3) 0.2500 -0.1122(2) 0.0567(7) Uani 1 2 d S . .
Cu1 Cu 0.73758(13) 0.67031(4) 0.29291(9) 0.0691(4) Uani 1 1 d . . .
Cu2 Cu 1.02137(17) 0.7500 0.18591(11) 0.0554(4) Uani 1 2 d S . .
Cu3 Cu 1.30569(17) 0.2500 0.05996(12) 0.0591(4) Uani 1 2 d S . .
N1 N 0.9134(8) 0.6201(3) 0.2425(5) 0.0556(16) Uani 1 1 d . . .
N2 N 1.0341(7) 0.6538(3) 0.1931(5) 0.0507(15) Uani 1 1 d . . .
N3 N 1.2783(8) 0.3440(3) 0.1073(5) 0.0514(15) Uani 1 1 d . . .
N4 N 0.5790(9) 0.7157(3) 0.3639(6) 0.070(2) Uani 1 1 d . . .
N5 N -0.0069(19) 0.7500 0.6623(12) 0.097(4) Uani 1 2 d S . .
C1 C 0.682(3) 0.4791(11) 0.2253(15) 0.107(8) Uani 0.50 1 d P . .
H1A H 0.6217 0.4485 0.2654 0.161 Uiso 0.50 1 calc PR . .
H1B H 0.7131 0.4549 0.1666 0.161 Uiso 0.50 1 calc PR . .
H1C H 0.6040 0.5168 0.2002 0.161 Uiso 0.50 1 calc PR . .
C1' C 0.870(4) 0.4946(13) 0.378(3) 0.187(18) Uani 0.50 1 d P . .
H1'A H 0.7876 0.4627 0.4002 0.280 Uiso 0.50 1 calc PR . .
H1'B H 0.8639 0.5377 0.4138 0.280 Uiso 0.50 1 calc PR . .
H1'C H 0.9900 0.4767 0.3958 0.280 Uiso 0.50 1 calc PR . .
C2 C 0.8314(13) 0.5031(4) 0.2863(8) 0.072(3) Uani 1 1 d . . .
C3 C 0.9459(9) 0.5521(3) 0.2393(6) 0.0526(19) Uani 1 1 d . . .
C4 C 1.0880(8) 0.5408(3) 0.1862(5) 0.0411(16) Uani 1 1 d . . .
C5 C 1.1390(8) 0.6072(3) 0.1576(5) 0.0438(16) Uani 1 1 d . . .
C6 C 1.2851(9) 0.6295(3) 0.1028(6) 0.0514(19) Uani 1 1 d . . .
H6A H 1.3697 0.5919 0.1040 0.062 Uiso 1 1 calc R . .
H6B H 1.3488 0.6675 0.1415 0.062 Uiso 1 1 calc R . .
C7 C 1.2213(12) 0.6514(4) -0.0100(7) 0.075(2) Uani 1 1 d . . .
H7A H 1.3226 0.6650 -0.0401 0.112 Uiso 1 1 calc R . .
H7B H 1.1399 0.6894 -0.0120 0.112 Uiso 1 1 calc R . .
H7C H 1.1607 0.6138 -0.0495 0.112 Uiso 1 1 calc R . .
C8 C 1.1609(8) 0.4748(3) 0.1610(6) 0.0439(16) Uani 1 1 d . . .
C9 C 1.1791(9) 0.4196(3) 0.2305(6) 0.0553(19) Uani 1 1 d . . .
H9A H 1.1541 0.4254 0.2977 0.066 Uiso 1 1 calc R . .
C10 C 1.2339(11) 0.3564(3) 0.2002(7) 0.061(2) Uani 1 1 d . . .
H10A H 1.2401 0.3202 0.2477 0.073 Uiso 1 1 calc R . .
C11 C 1.2685(9) 0.3976(3) 0.0406(6) 0.0475(17) Uani 1 1 d . . .
H11A H 1.3017 0.3911 -0.0244 0.057 Uiso 1 1 calc R . .
C12 C 1.2110(9) 0.4619(3) 0.0652(6) 0.0487(18) Uani 1 1 d . . .
H12A H 1.2059 0.4972 0.0163 0.058 Uiso 1 1 calc R . .
C13 C 0.499(2) 0.5970(8) 0.5218(11) 0.194(6) Uani 1 1 d . . .
H13A H 0.4711 0.5499 0.5336 0.291 Uiso 1 1 calc R . .
H13B H 0.4655 0.6252 0.5759 0.291 Uiso 1 1 calc R . .
H13C H 0.6259 0.6015 0.5233 0.291 Uiso 1 1 calc R . .
C14 C 0.4002(17) 0.6190(4) 0.4192(10) 0.130(4) Uani 1 1 d . . .
H14A H 0.2711 0.6157 0.4142 0.156 Uiso 1 1 calc R . .
H14B H 0.4364 0.5942 0.3615 0.156 Uiso 1 1 calc R . .
C15 C 0.4658(14) 0.6928(4) 0.4260(9) 0.095(3) Uani 1 1 d . . .
C16 C 0.3956(14) 0.7500 0.4693(10) 0.062(3) Uani 1 2 d S . .
C17 C 0.2589(15) 0.7500 0.5375(9) 0.064(3) Uani 1 2 d S . .
C18 C 0.0837(16) 0.7272(10) 0.4991(12) 0.088(9) Uani 0.50 1 d P . .
H18A H 0.0497 0.7104 0.4284 0.106 Uiso 0.50 1 d PR . .
C19 C -0.040(2) 0.7291(9) 0.5652(14) 0.081(7) Uani 0.50 1 d P . .
H19A H -0.1606 0.7142 0.5379 0.098 Uiso 0.50 1 d PR . .
C20 C 0.156(3) 0.7273(10) 0.6969(16) 0.107(9) Uani 0.50 1 d P . .
H20A H 0.1792 0.7056 0.7647 0.128 Uiso 0.50 1 d PR . .
C21 C 0.296(2) 0.7290(9) 0.6409(14) 0.090(8) Uani 0.50 1 d P . .
H21A H 0.4163 0.7172 0.6743 0.108 Uiso 0.50 1 d PR . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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
_geom_angle_publ_flag
N1 Cu1 N4 171.1(3) . . ?
N2 Cu2 N2 172.6(4) 4_575 . ?
N3 Cu3 N3 139.1(4) . 4_565 ?
N3 Cu3 Cl2 110.18(19) . . ?
N3 Cu3 Cl2 110.18(19) 4_565 . ?
C3 N1 N2 108.2(5) . . ?
C3 N1 Cu1 132.2(5) . . ?
N2 N1 Cu1 119.5(4) . . ?
C5 N2 N1 108.9(5) . . ?
C5 N2 Cu2 133.3(5) . . ?
N1 N2 Cu2 117.8(4) . . ?
C10 N3 C11 116.5(6) . . ?
C10 N3 Cu3 120.8(5) . . ?
C11 N3 Cu3 121.5(5) . . ?
N4 N4 C15 109.2(4) 4_575 . ?
N4 N4 Cu1 118.31(17) 4_575 . ?
C15 N4 Cu1 132.3(5) . . ?
C19 N5 C19 36.5(16) . 4_575 ?
C19 N5 C20 115.9(14) . 4_575 ?
C19 N5 C20 103.0(14) 4_575 4_575 ?
C19 N5 C20 103.0(14) . . ?
C19 N5 C20 115.9(14) 4_575 . ?
C20 N5 C20 39.4(19) 4_575 . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C2 C1' H1'A 109.5 . . ?
C2 C1' H1'B 109.5 . . ?
H1'A C1' H1'B 109.5 . . ?
C2 C1' H1'C 109.5 . . ?
H1'A C1' H1'C 109.5 . . ?
H1'B C1' H1'C 109.5 . . ?
C1' C2 C1 124.7(18) . . ?
C1' C2 C3 116.4(17) . . ?
C1 C2 C3 118.3(11) . . ?
N1 C3 C4 109.4(6) . . ?
N1 C3 C2 119.5(6) . . ?
C4 C3 C2 131.1(6) . . ?
C3 C4 C5 104.9(5) . . ?
C3 C4 C8 127.3(6) . . ?
C5 C4 C8 127.8(6) . . ?
N2 C5 C4 108.7(6) . . ?
N2 C5 C6 120.4(5) . . ?
C4 C5 C6 130.8(6) . . ?
C5 C6 C7 114.2(6) . . ?
C5 C6 H6A 108.7 . . ?
C7 C6 H6A 108.7 . . ?
C5 C6 H6B 108.7 . . ?
C7 C6 H6B 108.7 . . ?
H6A C6 H6B 107.6 . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C12 C8 C9 115.3(6) . . ?
C12 C8 C4 122.5(6) . . ?
C9 C8 C4 122.2(6) . . ?
C10 C9 C8 120.3(7) . . ?
C10 C9 H9A 119.8 . . ?
C8 C9 H9A 119.8 . . ?
N3 C10 C9 123.9(7) . . ?
N3 C10 H10A 118.0 . . ?
C9 C10 H10A 118.0 . . ?
N3 C11 C12 122.5(6) . . ?
N3 C11 H11A 118.8 . . ?
C12 C11 H11A 118.8 . . ?
C11 C12 C8 121.4(6) . . ?
C11 C12 H12A 119.3 . . ?
C8 C12 H12A 119.3 . . ?
C14 C13 H13A 109.5 . . ?
C14 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C14 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C13 C14 C15 96.7(10) . . ?
C13 C14 H14A 112.4 . . ?
C15 C14 H14A 112.4 . . ?
C13 C14 H14B 112.4 . . ?
C15 C14 H14B 112.4 . . ?
H14A C14 H14B 110.0 . . ?
N4 C15 C16 107.8(7) . . ?
N4 C15 C14 120.9(8) . . ?
C16 C15 C14 129.3(8) . . ?
C15 C16 C15 105.9(10) 4_575 . ?
C15 C16 C17 126.9(5) 4_575 . ?
C15 C16 C17 126.9(5) . . ?
C21 C17 C21 34.6(16) 4_575 . ?
C21 C17 C18 116.6(13) 4_575 . ?
C21 C17 C18 105.0(12) . . ?
C21 C17 C18 105.0(12) 4_575 4_575 ?
C21 C17 C18 116.6(13) . 4_575 ?
C18 C17 C18 37.0(16) . 4_575 ?
C21 C17 C16 122.7(12) 4_575 . ?
C21 C17 C16 122.7(12) . . ?
C18 C17 C16 120.7(10) . . ?
C18 C17 C16 120.7(10) 4_575 . ?
C18 C18 C19 88.5(11) 4_575 . ?
C18 C18 C17 71.5(8) 4_575 . ?
C19 C18 C17 118.7(14) . . ?
C18 C18 C19 58.3(8) 4_575 4_575 ?
C19 C18 C19 30.1(13) . 4_575 ?
C17 C18 C19 104.4(13) . 4_575 ?
C18 C18 H18A 109.9 4_575 . ?
C19 C18 H18A 120.4 . . ?
C17 C18 H18A 121.0 . . ?
C19 C18 H18A 127.0 4_575 . ?
C19 C19 N5 71.7(8) 4_575 . ?
C19 C19 C18 91.5(11) 4_575 . ?
N5 C19 C18 125.1(16) . . ?
C19 C19 C18 58.3(8) 4_575 4_575 ?
N5 C19 C18 108.5(14) . 4_575 ?
C18 C19 C18 33.2(14) . 4_575 ?
C19 C19 H19A 107.5 4_575 . ?
N5 C19 H19A 116.7 . . ?
C18 C19 H19A 118.2 . . ?
C18 C19 H19A 124.5 4_575 . ?
C20 C20 N5 70.3(9) 4_575 . ?
C20 C20 C21 88.7(11) 4_575 . ?
N5 C20 C21 125.1(17) . . ?
C20 C20 C21 58.5(9) 4_575 4_575 ?
N5 C20 C21 108.7(15) . 4_575 ?
C21 C20 C21 30.2(14) . 4_575 ?
C20 C20 H20A 116.2 4_575 . ?
N5 C20 H20A 117.4 . . ?
C21 C20 H20A 117.4 . . ?
C21 C20 H20A 127.9 4_575 . ?
C21 C21 C17 72.7(8) 4_575 . ?
C21 C21 C20 91.3(11) 4_575 . ?
C17 C21 C20 118.4(17) . . ?
C21 C21 C20 58.5(9) 4_575 4_575 ?
C17 C21 C20 104.1(14) . 4_575 ?
C20 C21 C20 32.8(15) . 4_575 ?
C21 C21 H21A 103.7 4_575 . ?
C17 C21 H21A 120.9 . . ?
C20 C21 H21A 120.7 . . ?
C20 C21 H21A 124.4 4_575 . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cl2 Cu3 2.317(3) . ?
Cu1 N1 1.864(5) . ?
Cu1 N4 1.864(6) . ?
Cu2 N2 1.877(5) 4_575 ?
Cu2 N2 1.877(5) . ?
Cu3 N3 1.954(5) . ?
Cu3 N3 1.954(5) 4_565 ?
N1 C3 1.349(8) . ?
N1 N2 1.375(7) . ?
N2 C5 1.342(8) . ?
N3 C10 1.328(9) . ?
N3 C11 1.347(8) . ?
N4 N4 1.335(11) 4_575 ?
N4 C15 1.354(9) . ?
N5 C19 1.299(18) . ?
N5 C19 1.299(18) 4_575 ?
N5 C20 1.31(2) 4_575 ?
N5 C20 1.31(2) . ?
C1 C2 1.337(18) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C1' C2 1.18(3) . ?
C1' H1'A 0.9600 . ?
C1' H1'B 0.9600 . ?
C1' H1'C 0.9600 . ?
C2 C3 1.493(10) . ?
C3 C4 1.398(9) . ?
C4 C5 1.417(8) . ?
C4 C8 1.459(8) . ?
C5 C6 1.485(9) . ?
C6 C7 1.511(11) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 C12 1.384(9) . ?
C8 C9 1.391(9) . ?
C9 C10 1.379(9) . ?
C9 H9A 0.9300 . ?
C10 H10A 0.9300 . ?
C11 C12 1.380(8) . ?
C11 H11A 0.9300 . ?
C12 H12A 0.9300 . ?
C13 C14 1.461(7) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 C15 1.518(7) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 C16 1.394(10) . ?
C16 C15 1.394(10) 4_575 ?
C16 C17 1.480(14) . ?
C17 C21 1.377(19) 4_575 ?
C17 C21 1.377(19) . ?
C17 C18 1.399(9) . ?
C17 C18 1.399(9) 4_575 ?
C18 C18 0.89(4) 4_575 ?
C18 C19 1.381(9) . ?
C18 C19 1.622(15) 4_575 ?
C18 H18A 0.9599 . ?
C19 C19 0.81(3) 4_575 ?
C19 C18 1.622(15) 4_575 ?
C19 H19A 0.9600 . ?
C20 C20 0.88(4) 4_575 ?
C20 C21 1.39(2) . ?
C20 C21 1.63(2) 4_575 ?
C20 H20A 0.9600 . ?
C21 C21 0.82(4) 4_575 ?
C21 C20 1.63(2) 4_575 ?
C21 H21A 0.9601 . ?
