#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:43:37 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179344 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/41/4324127.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_4324127
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 Br Cu4 N9'
_chemical_formula_weight         934.86
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/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                 112.943(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.060(6)
_cell_length_b                   19.446(7)
_cell_length_c                   14.059(8)
_cell_measurement_reflns_used    1802
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      22.98
_cell_measurement_theta_min      2.74
_cell_volume                     3792(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.0725
_diffrn_reflns_av_sigmaI/netI    0.1054
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9849
_diffrn_reflns_theta_full        25.98
_diffrn_reflns_theta_max         25.98
_diffrn_reflns_theta_min         1.98
_exptl_absorpt_coefficient_mu    3.306
_exptl_absorpt_correction_T_max  0.7334
_exptl_absorpt_correction_T_min  0.5876
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.638
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1888
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.015
_refine_diff_density_min         -0.587
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         3797
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.1177
_refine_ls_R_factor_gt           0.0610
_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)+(0.0687P)²+6.3624P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1533
_refine_ls_wR_factor_ref         0.1759
_reflns_number_gt                2110
_reflns_number_total             3797
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic101901w_si_002_2.cif
_cod_data_source_block           complex_2
_cod_original_cell_volume        3791(3)
_cod_database_code               4324127
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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
Br1 Br 0.48471(8) 0.0000 0.14089(9) 0.0502(3) Uani 1 2 d S . .
Cu3 Cu 0.39345(10) 0.0000 -0.05095(12) 0.0547(4) Uani 1 2 d S . .
Cu2 Cu 0.31966(9) 0.0000 0.20190(11) 0.0490(4) Uani 1 2 d S . .
Cu1 Cu 0.51460(6) 0.07956(5) 0.32457(8) 0.0552(3) Uani 1 1 d . . .
N1 N 0.4016(4) 0.1297(3) 0.2596(5) 0.0478(16) Uani 1 1 d . . .
N2 N 0.3167(4) 0.0966(3) 0.2070(5) 0.0443(15) Uani 1 1 d . . .
N3 N 0.1598(4) 0.4070(3) 0.0914(5) 0.0521(17) Uani 1 1 d . . .
N4 N 0.6286(4) 0.0354(3) 0.4048(5) 0.0574(19) Uani 1 1 d . . .
N5 N 1.0733(12) 0.0000 0.7083(11) 0.150(8) Uani 1 2 d S . .
C1 C 0.5220(9) 0.2558(7) 0.2322(9) 0.138(5) Uani 1 1 d . . .
H1A H 0.5731 0.2880 0.2650 0.207 Uiso 1 1 calc R . .
H1B H 0.4807 0.2730 0.1656 0.207 Uiso 1 1 calc R . .
H1C H 0.5489 0.2125 0.2242 0.207 Uiso 1 1 calc R . .
C2 C 0.4653(6) 0.2463(4) 0.2969(7) 0.065(2) Uani 1 1 d . . .
H2A H 0.4396 0.2903 0.3065 0.077 Uiso 1 1 calc R . .
H2B H 0.5072 0.2292 0.3643 0.077 Uiso 1 1 calc R . .
C3 C 0.3843(5) 0.1970(4) 0.2482(6) 0.0461(19) Uani 1 1 d . . .
C4 C 0.2871(5) 0.2086(4) 0.1867(5) 0.0399(17) Uani 1 1 d . . .
C5 C 0.2490(5) 0.1435(4) 0.1626(6) 0.0435(18) Uani 1 1 d . . .
C6 C 0.1467(5) 0.1205(5) 0.0987(7) 0.062(2) Uani 1 1 d . . .
H6A H 0.1030 0.1581 0.0943 0.074 Uiso 1 1 calc R . .
H6B H 0.1304 0.0827 0.1339 0.074 Uiso 1 1 calc R . .
C7 C 0.1310(7) 0.0975(6) -0.0109(8) 0.091(3) Uani 1 1 d . . .
H7A H 0.0651 0.0837 -0.0468 0.136 Uiso 1 1 calc R . .
H7B H 0.1728 0.0595 -0.0074 0.136 Uiso 1 1 calc R . .
H7C H 0.1453 0.1350 -0.0471 0.136 Uiso 1 1 calc R . .
C8 C 0.2406(5) 0.2757(4) 0.1547(6) 0.0431(18) Uani 1 1 d . . .
C9 C 0.2586(6) 0.3302(4) 0.2210(7) 0.060(2) Uani 1 1 d . . .
H9 H 0.2987 0.3242 0.2901 0.072 Uiso 1 1 calc R . .
C10 C 0.2194(6) 0.3928(4) 0.1882(7) 0.064(3) Uani 1 1 d . . .
H10 H 0.2349 0.4282 0.2363 0.077 Uiso 1 1 calc R . .
C11 C 0.1383(5) 0.3541(4) 0.0256(6) 0.051(2) Uani 1 1 d . . .
H11 H 0.0964 0.3614 -0.0425 0.061 Uiso 1 1 calc R . .
C12 C 0.1758(5) 0.2884(4) 0.0545(6) 0.050(2) Uani 1 1 d . . .
H12 H 0.1573 0.2528 0.0065 0.059 Uiso 1 1 calc R . .
C13 C 0.7109(9) 0.1610(6) 0.5627(8) 0.101(4) Uani 1 1 d . . .
H13A H 0.7252 0.2093 0.5700 0.151 Uiso 1 1 calc R . .
H13B H 0.7479 0.1380 0.6263 0.151 Uiso 1 1 calc R . .
H13C H 0.6435 0.1541 0.5464 0.151 Uiso 1 1 calc R . .
C14 C 0.7354(6) 0.1333(4) 0.4807(6) 0.061(2) Uani 1 1 d . . .
H14A H 0.8031 0.1421 0.4964 0.074 Uiso 1 1 calc R . .
H14B H 0.6980 0.1569 0.4168 0.074 Uiso 1 1 calc R . .
C15 C 0.7166(5) 0.0565(4) 0.4655(6) 0.050(2) Uani 1 1 d . . .
C16 C 0.7761(8) 0.0000 0.5074(9) 0.065(4) Uani 1 2 d S . .
C17 C 0.8778(8) 0.0000 0.5760(10) 0.082(5) Uani 1 2 d SD . .
C18 C 0.9414(10) -0.0470(7) 0.5599(13) 0.089(8) Uani 0.451(16) 1 d PD . 1
H18A H 0.9198 -0.0784 0.5058 0.106 Uiso 0.451(16) 1 calc PR . 1
C19 C 1.0384(12) -0.0451(7) 0.6280(13) 0.091(8) Uani 0.451(16) 1 d PD . 1
H19A H 1.0810 -0.0760 0.6179 0.109 Uiso 0.451(16) 1 calc PR . 1
C19' C 1.0129(11) 0.0433(8) 0.7227(14) 0.149(10) Uani 0.549(16) 1 d PD . 2
H19B H 1.0359 0.0741 0.7776 0.178 Uiso 0.549(16) 1 calc PR . 2
C18' C 0.9170(12) 0.0445(7) 0.6592(11) 0.142(10) Uani 0.549(16) 1 d PD . 2
H18B H 0.8769 0.0762 0.6722 0.171 Uiso 0.549(16) 1 calc PR . 2
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'
Br Br -0.2901 2.4595 '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
Cu3 Br1 Cu3 70.84(7) . 5_655 ?
Cu3 Br1 Cu1 142.27(4) . . ?
Cu3 Br1 Cu1 122.69(5) 5_655 . ?
Cu3 Br1 Cu1 142.27(4) . 6 ?
Cu3 Br1 Cu1 122.69(5) 5_655 6 ?
Cu1 Br1 Cu1 64.70(6) . 6 ?
N3 Cu3 N3 133.2(4) 4_545 7 ?
N3 Cu3 Br1 107.54(19) 4_545 . ?
N3 Cu3 Br1 107.54(19) 7 . ?
N3 Cu3 Br1 98.3(2) 4_545 5_655 ?
N3 Cu3 Br1 98.3(2) 7 5_655 ?
Br1 Cu3 Br1 109.16(7) . 5_655 ?
N3 Cu3 Cu3 112.48(19) 4_545 5_655 ?
N3 Cu3 Cu3 112.48(19) 7 5_655 ?
Br1 Cu3 Cu3 56.13(5) . 5_655 ?
Br1 Cu3 Cu3 53.03(6) 5_655 5_655 ?
N2 Cu2 N2 174.1(4) 6 . ?
N4 Cu1 N1 172.6(3) . . ?
N4 Cu1 Br1 94.6(2) . . ?
N1 Cu1 Br1 92.73(19) . . ?
C3 N1 N2 107.5(6) . . ?
C3 N1 Cu1 132.2(5) . . ?
N2 N1 Cu1 120.2(4) . . ?
C5 N2 N1 108.4(6) . . ?
C5 N2 Cu2 133.9(5) . . ?
N1 N2 Cu2 117.5(4) . . ?
C10 N3 C11 115.5(7) . . ?
C10 N3 Cu3 121.4(6) . 7 ?
C11 N3 Cu3 123.1(5) . 7 ?
C15 N4 N4 107.9(4) . 6 ?
C15 N4 Cu1 134.5(6) . . ?
N4 N4 Cu1 117.5(2) 6 . ?
C19' N5 C19' 80.0(14) 6 . ?
C19' N5 C19 69.4(12) 6 . ?
C19' N5 C19 118.4(18) . . ?
C19' N5 C19 118.4(18) 6 6 ?
C19' N5 C19 69.4(12) . 6 ?
C19 N5 C19 80.1(13) . 6 ?
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 . . ?
C1 C2 C3 111.2(8) . . ?
C1 C2 H2A 109.4 . . ?
C3 C2 H2A 109.4 . . ?
C1 C2 H2B 109.4 . . ?
C3 C2 H2B 109.4 . . ?
H2A C2 H2B 108.0 . . ?
N1 C3 C4 110.0(7) . . ?
N1 C3 C2 119.3(7) . . ?
C4 C3 C2 130.6(7) . . ?
C5 C4 C3 103.8(6) . . ?
C5 C4 C8 129.8(7) . . ?
C3 C4 C8 126.4(7) . . ?
N2 C5 C4 110.3(6) . . ?
N2 C5 C6 119.5(7) . . ?
C4 C5 C6 130.3(7) . . ?
C5 C6 C7 113.8(7) . . ?
C5 C6 H6A 108.8 . . ?
C7 C6 H6A 108.8 . . ?
C5 C6 H6B 108.8 . . ?
C7 C6 H6B 108.8 . . ?
H6A C6 H6B 107.7 . . ?
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 . . ?
C9 C8 C12 115.4(7) . . ?
C9 C8 C4 122.5(7) . . ?
C12 C8 C4 122.2(7) . . ?
C10 C9 C8 121.4(8) . . ?
C10 C9 H9 119.3 . . ?
C8 C9 H9 119.3 . . ?
N3 C10 C9 124.4(8) . . ?
N3 C10 H10 117.8 . . ?
C9 C10 H10 117.8 . . ?
N3 C11 C12 122.9(7) . . ?
N3 C11 H11 118.5 . . ?
C12 C11 H11 118.5 . . ?
C8 C12 C11 120.3(8) . . ?
C8 C12 H12 119.9 . . ?
C11 C12 H12 119.9 . . ?
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 112.8(8) . . ?
C13 C14 H14A 109.0 . . ?
C15 C14 H14A 109.0 . . ?
C13 C14 H14B 109.0 . . ?
C15 C14 H14B 109.0 . . ?
H14A C14 H14B 107.8 . . ?
N4 C15 C16 110.1(7) . . ?
N4 C15 C14 118.5(7) . . ?
C16 C15 C14 131.4(7) . . ?
C15 C16 C15 104.0(9) 6 . ?
C15 C16 C17 128.0(5) 6 . ?
C15 C16 C17 128.0(5) . . ?
C18' C17 C18' 77.2(12) . 6 ?
C18' C17 C18 116.6(13) . . ?
C18' C17 C18 68.7(11) 6 . ?
C18' C17 C18 68.7(11) . 6 ?
C18' C17 C18 116.6(14) 6 6 ?
C18 C17 C18 81.2(13) . 6 ?
C18' C17 C16 123.4(11) . . ?
C18' C17 C16 123.4(11) 6 . ?
C18 C17 C16 120.0(10) . . ?
C18 C17 C16 120.0(10) 6 . ?
C19 C18 C17 118.0(16) . . ?
C19 C18 C18 88.5(7) . 6 ?
C17 C18 C18 49.4(6) . 6 ?
C19 C18 H18A 121.0 . . ?
C17 C18 H18A 121.0 . . ?
C18 C18 H18A 131.0 6 . ?
N5 C19 C18 123.0(18) . . ?
N5 C19 C19 50.0(6) . 6 ?
C18 C19 C19 91.5(7) . 6 ?
N5 C19 H19A 118.5 . . ?
C18 C19 H19A 118.5 . . ?
C19 C19 H19A 130.3 6 . ?
N5 C19' C18' 121.9(19) . . ?
N5 C19' C19' 50.0(7) . 6 ?
C18' C19' C19' 91.0(7) . 6 ?
N5 C19' H19B 119.1 . . ?
C18' C19' H19B 119.1 . . ?
C19' C19' H19B 130.1 6 . ?
C19' C18' C17 122.2(17) . . ?
C19' C18' C18' 89.0(7) . 6 ?
C17 C18' C18' 51.4(6) . 6 ?
C19' C18' H18B 118.9 . . ?
C17 C18' H18B 118.9 . . ?
C18' C18' H18B 131.5 6 . ?
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
Br1 Cu3 2.505(2) . ?
Br1 Cu3 2.603(2) 5_655 ?
Br1 Cu1 2.8910(19) . ?
Br1 Cu1 2.8910(19) 6 ?
Cu3 N3 1.970(6) 4_545 ?
Cu3 N3 1.970(6) 7 ?
Cu3 Br1 2.603(2) 5_655 ?
Cu3 Cu3 2.961(3) 5_655 ?
Cu2 N2 1.881(6) 6 ?
Cu2 N2 1.881(6) . ?
Cu1 N4 1.856(6) . ?
Cu1 N1 1.862(6) . ?
N1 C3 1.331(9) . ?
N1 N2 1.364(8) . ?
N2 C5 1.329(9) . ?
N3 C10 1.335(10) . ?
N3 C11 1.337(10) . ?
N3 Cu3 1.970(6) 7 ?
N4 C15 1.332(9) . ?
N4 N4 1.377(13) 6 ?
N5 C19' 1.311(10) 6 ?
N5 C19' 1.311(10) . ?
N5 C19 1.363(10) . ?
N5 C19 1.363(10) 6 ?
C1 C2 1.482(9) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 C3 1.492(10) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.399(10) . ?
C4 C5 1.377(10) . ?
C4 C8 1.465(10) . ?
C5 C6 1.518(11) . ?
C6 C7 1.531(13) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 C9 1.367(10) . ?
C8 C12 1.387(10) . ?
C9 C10 1.352(11) . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
C11 C12 1.392(10) . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
C13 C14 1.445(13) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 C15 1.519(11) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 C16 1.395(10) . ?
C16 C15 1.395(10) 6 ?
C16 C17 1.457(15) . ?
C17 C18' 1.389(8) . ?
C17 C18' 1.389(8) 6 ?
C17 C18 1.404(8) . ?
C17 C18 1.404(8) 6 ?
C18 C19 1.401(10) . ?
C18 H18A 0.9300 . ?
C19 H19A 0.9300 . ?
C19' C18' 1.371(10) . ?
C19' H19B 0.9300 . ?
C18' H18B 0.9300 . ?
