#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:30:40 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179114 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/76/4307630.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_4307630
loop_
_publ_author_name
'Alok Ranjan Paital'
'A-Qing Wu'
'Guo-Cong Guo'
'Guillem Aromí'
'Jordi Ribas-Ariño'
'Debashis Ray'
_publ_contact_author_address
;Debashis Ray 
 Department of Chemistry
 Indian Institute of Technology
 Kharagpur-721302
 India
;
_publ_contact_author_email       dray@chem.iitkgp.ernet.in
_publ_contact_author_fax         91-3222-255303
_publ_contact_author_name        'Dr. Debashis Ray'
_publ_contact_author_phone       ' 03222-283324'
_publ_section_title
;
Two Cu2 and Zn2 Metallamacrocycles Featuring a Novel Extended π-Conjugated
Carbazole Bridge
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2947
_journal_page_last               2949
_journal_paper_doi               10.1021/ic062109z
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C27 H20 Cl3 Cu N3 O3'
_chemical_formula_weight         604.35
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                78.153(19)
_cell_angle_beta                 68.288(14)
_cell_angle_gamma                65.790(15)
_cell_formula_units_Z            2
_cell_length_a                   10.5504(5)
_cell_length_b                   11.837
_cell_length_c                   11.92530(10)
_cell_measurement_reflns_used    3325
_cell_measurement_temperature    3273(2)
_cell_measurement_theta_max      27.4835
_cell_measurement_theta_min      3.3178
_cell_volume                     1259.42(19)
_computing_cell_refinement       'CrystalClear (Rigaku Corp., 2002)'
_computing_data_collection       'CrystalClear (Rigaku Corp., 2002)'
_computing_data_reduction        'CrystalClear (Rigaku Corp., 2002)'
_computing_publication_material  'Siemens SHELXTLTM 5'
_computing_structure_refinement  'Siemens SHELXTLTM 5'
_computing_structure_solution    'Siemens SHELXTLTM 5'
_diffrn_ambient_temperature      3273(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Rigaku Mercury CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating-anode generator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0230
_diffrn_reflns_av_sigmaI/netI    0.0409
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9920
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.32
_exptl_absorpt_coefficient_mu    1.222
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6439
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrystalClear, Rigaku 2002)'
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.594
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             614
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.025
_refine_diff_density_min         -1.092
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         5666
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0836
_refine_ls_R_factor_gt           0.0713
_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)+(0.1363P)²+1.1402P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1992
_refine_ls_wR_factor_ref         0.2152
_reflns_number_gt                4631
_reflns_number_total             5666
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic062109z-file003.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        1259.43(6)
_cod_database_code               4307630
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.24508(5) -0.29160(4) 0.33328(4) 0.03538(19) Uani 1 1 d . . .
O2 O -0.4433(3) 0.3589(3) -0.3370(3) 0.0435(7) Uani 1 1 d . . .
O1 O 0.1616(3) -0.3362(3) 0.4965(3) 0.0428(7) Uani 1 1 d . . .
N3 N -0.2723(3) 0.1520(3) -0.2191(3) 0.0355(7) Uani 1 1 d . . .
N1 N 0.1053(3) -0.3108(3) 0.2750(3) 0.0352(7) Uani 1 1 d . . .
C13 C 0.0391(4) -0.2118(3) 0.0914(3) 0.0316(7) Uani 1 1 d . . .
H13A H -0.0513 -0.1589 0.1372 0.038 Uiso 1 1 calc R . .
N2 N 0.2350(4) -0.2575(3) -0.2237(3) 0.0425(8) Uani 1 1 d . . .
H2B H 0.3092 -0.2963 -0.2819 0.051 Uiso 1 1 calc R . .
C12 C 0.0812(4) -0.2033(3) -0.0350(3) 0.0301(7) Uani 1 1 d . . .
C1 C 0.0305(4) -0.3423(4) 0.5443(3) 0.0352(8) Uani 1 1 d . . .
C14 C 0.0141(4) -0.1196(3) -0.1217(3) 0.0316(7) Uani 1 1 d . . .
Cl3 Cl1 0.6608(4) -0.0345(4) -0.3586(4) 0.1928(19) Uani 1 1 d . . .
C19 C -0.1165(4) -0.0183(3) -0.1122(3) 0.0328(7) Uani 1 1 d . . .
H19A H -0.1846 0.0060 -0.0369 0.039 Uiso 1 1 calc R . .
C26 C -0.5538(4) 0.3438(4) -0.2447(3) 0.0367(8) Uani 1 1 d . . .
C11 C 0.2169(4) -0.2866(4) -0.1032(3) 0.0369(8) Uani 1 1 d . . .
C20 C -0.3987(4) 0.1553(4) -0.1460(3) 0.0383(8) Uani 1 1 d . . .
H20A H -0.4010 0.0900 -0.0877 0.046 Uiso 1 1 calc R . .
C18 C -0.1434(4) 0.0461(3) -0.2177(3) 0.0339(7) Uani 1 1 d . . .
C8 C 0.1359(4) -0.3015(4) 0.1466(3) 0.0340(7) Uani 1 1 d . . .
C6 C -0.0577(4) -0.3379(4) 0.4762(3) 0.0365(8) Uani 1 1 d . . .
C7 C -0.0127(4) -0.3270(4) 0.3462(3) 0.0352(8) Uani 1 1 d . . .
H7A H -0.0747 -0.3321 0.3104 0.042 Uiso 1 1 calc R . .
C9 C 0.2715(4) -0.3827(4) 0.0780(4) 0.0426(9) Uani 1 1 d . . .
H9A H 0.3349 -0.4411 0.1173 0.051 Uiso 1 1 calc R . .
C16 C 0.0890(5) -0.0914(4) -0.3427(3) 0.0427(9) Uani 1 1 d . . .
H16A H 0.1559 -0.1161 -0.4182 0.051 Uiso 1 1 calc R . .
C21 C -0.5377(4) 0.2520(4) -0.1468(4) 0.0387(8) Uani 1 1 d . . .
C25 C -0.6978(4) 0.4206(4) -0.2426(4) 0.0426(9) Uani 1 1 d . . .
H25A H -0.7125 0.4785 -0.3068 0.051 Uiso 1 1 calc R . .
C15 C 0.1148(4) -0.1556(4) -0.2369(3) 0.0366(8) Uani 1 1 d . . .
C3 C -0.1617(5) -0.3668(5) 0.7265(4) 0.0493(10) Uani 1 1 d . . .
H3A H -0.1953 -0.3781 0.8104 0.059 Uiso 1 1 calc R . .
C17 C -0.0384(5) 0.0096(4) -0.3313(3) 0.0423(9) Uani 1 1 d . . .
H17A H -0.0565 0.0556 -0.4007 0.051 Uiso 1 1 calc R . .
C2 C -0.0285(5) -0.3528(4) 0.6705(4) 0.0447(9) Uani 1 1 d . . .
H2A H 0.0234 -0.3502 0.7176 0.054 Uiso 1 1 calc R . .
C23 C -0.8013(5) 0.3247(5) -0.0498(4) 0.0503(10) Uani 1 1 d . . .
H23A H -0.8828 0.3212 0.0152 0.060 Uiso 1 1 calc R . .
C24 C -0.8174(4) 0.4115(5) -0.1468(4) 0.0480(10) Uani 1 1 d . . .
H24A H -0.9111 0.4648 -0.1471 0.058 Uiso 1 1 calc R . .
C5 C -0.1929(5) -0.3517(4) 0.5360(4) 0.0444(9) Uani 1 1 d . . .
H5A H -0.2480 -0.3524 0.4909 0.053 Uiso 1 1 calc R . .
C10 C 0.3128(5) -0.3777(4) -0.0460(4) 0.0470(10) Uani 1 1 d . . .
H10A H 0.4018 -0.4332 -0.0907 0.056 Uiso 1 1 calc R . .
C22 C -0.6618(5) 0.2439(4) -0.0521(4) 0.0461(10) Uani 1 1 d . . .
H22A H -0.6501 0.1831 0.0104 0.055 Uiso 1 1 calc R . .
Cl2 Cl1 0.4448(4) -0.1063(4) -0.1731(3) 0.1763(16) Uani 1 1 d . . .
C4 C -0.2460(5) -0.3645(5) 0.6603(4) 0.0484(10) Uani 1 1 d . . .
H4A H -0.3371 -0.3714 0.6990 0.058 Uiso 1 1 calc R . .
C27 C 0.4992(9) -0.0299(12) -0.3225(7) 0.130(4) Uani 1 1 d . . .
H27A H 0.5115 -0.0896 -0.3754 0.156 Uiso 1 1 calc R . .
Cl1 Cl1 0.3624(6) 0.0855(5) -0.3439(5) 0.241(3) Uani 1 1 d . . .
O1W O -0.4791(4) 0.3766(3) 0.4252(3) 0.0543(8) Uani 1 1 d . . .
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'
O O 0.0106 0.0060 '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 Cl1 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
O1 Cu1 O2 95.27(12) . 2 ?
O1 Cu1 N1 95.98(13) . . ?
O2 Cu1 N1 145.63(14) 2 . ?
O1 Cu1 N3 143.85(14) . 2 ?
O2 Cu1 N3 94.02(13) 2 2 ?
N1 Cu1 N3 95.75(13) . 2 ?
C26 O2 Cu1 122.6(2) . 2 ?
C1 O1 Cu1 125.1(2) . . ?
C20 N3 C18 120.7(3) . . ?
C20 N3 Cu1 122.6(3) . 2 ?
C18 N3 Cu1 116.7(3) . 2 ?
C7 N1 C8 120.0(3) . . ?
C7 N1 Cu1 122.9(3) . . ?
C8 N1 Cu1 117.1(2) . . ?
C8 C13 C12 118.2(3) . . ?
C11 N2 C15 108.9(3) . . ?
C13 C12 C11 120.4(3) . . ?
C13 C12 C14 133.4(3) . . ?
C11 C12 C14 106.2(3) . . ?
O1 C1 C2 118.5(4) . . ?
O1 C1 C6 124.3(3) . . ?
C2 C1 C6 117.1(4) . . ?
C19 C14 C15 119.7(3) . . ?
C19 C14 C12 134.2(3) . . ?
C15 C14 C12 106.1(3) . . ?
C14 C19 C18 118.7(3) . . ?
O2 C26 C25 118.5(4) . . ?
O2 C26 C21 124.3(3) . . ?
C25 C26 C21 117.1(4) . . ?
N2 C11 C10 129.7(4) . . ?
N2 C11 C12 109.5(3) . . ?
C10 C11 C12 120.8(3) . . ?
N3 C20 C21 125.5(4) . . ?
C19 C18 C17 120.1(3) . . ?
C19 C18 N3 123.6(3) . . ?
C17 C18 N3 116.2(3) . . ?
C13 C8 C9 121.1(3) . . ?
C13 C8 N1 121.5(3) . . ?
C9 C8 N1 117.3(3) . . ?
C5 C6 C1 119.7(4) . . ?
C5 C6 C7 116.5(4) . . ?
C1 C6 C7 123.7(4) . . ?
N1 C7 C6 126.1(3) . . ?
C10 C9 C8 121.5(3) . . ?
C17 C16 C15 117.4(4) . . ?
C22 C21 C26 120.1(4) . . ?
C22 C21 C20 116.4(4) . . ?
C26 C21 C20 123.1(4) . . ?
C24 C25 C26 121.1(4) . . ?
N2 C15 C16 128.8(4) . . ?
N2 C15 C14 109.3(3) . . ?
C16 C15 C14 121.9(3) . . ?
C2 C3 C4 121.1(4) . . ?
C16 C17 C18 122.1(4) . . ?
C3 C2 C1 121.5(4) . . ?
C22 C23 C24 118.6(4) . . ?
C25 C24 C23 121.6(4) . . ?
C4 C5 C6 121.4(4) . . ?
C9 C10 C11 118.1(4) . . ?
C23 C22 C21 121.2(4) . . ?
C5 C4 C3 118.9(4) . . ?
Cl3 C27 Cl1 126.4(9) . . ?
Cl3 C27 Cl2 111.2(5) . . ?
Cl1 C27 Cl2 110.1(5) . . ?
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
Cu1 O1 1.880(3) . ?
Cu1 O2 1.923(3) 2 ?
Cu1 N1 1.952(3) . ?
Cu1 N3 1.960(3) 2 ?
O2 C26 1.320(5) . ?
O2 Cu1 1.923(3) 2 ?
O1 C1 1.313(5) . ?
N3 C20 1.285(5) . ?
N3 C18 1.426(5) . ?
N3 Cu1 1.960(3) 2 ?
N1 C7 1.286(5) . ?
N1 C8 1.433(5) . ?
C13 C8 1.387(5) . ?
C13 C12 1.400(5) . ?
N2 C11 1.367(5) . ?
N2 C15 1.379(5) . ?
C12 C11 1.412(5) . ?
C12 C14 1.449(5) . ?
C1 C2 1.400(5) . ?
C1 C6 1.424(5) . ?
C14 C19 1.391(5) . ?
C14 C15 1.409(5) . ?
Cl3 C27 1.577(10) . ?
C19 C18 1.391(5) . ?
C26 C25 1.408(5) . ?
C26 C21 1.431(5) . ?
C11 C10 1.402(5) . ?
C20 C21 1.445(5) . ?
C18 C17 1.409(5) . ?
C8 C9 1.403(5) . ?
C6 C5 1.401(6) . ?
C6 C7 1.438(5) . ?
C9 C10 1.374(6) . ?
C16 C17 1.367(6) . ?
C16 C15 1.390(5) . ?
C21 C22 1.402(6) . ?
C25 C24 1.379(6) . ?
C3 C2 1.379(7) . ?
C3 C4 1.380(7) . ?
C23 C22 1.381(6) . ?
C23 C24 1.392(7) . ?
C5 C4 1.377(6) . ?
Cl2 C27 1.824(10) . ?
C27 Cl1 1.589(10) . ?
