#------------------------------------------------------------------------------
#$Date: 2017-07-29 04:10:52 +0200 (Sat 29 de Jul de 2017) $
#$Revision: 199394 $
#$URL: svn://www.crystallography.net/cod/cif/7/22/87/7228799.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_7228799
loop_
_publ_author_name
'Avasthi, Ilesha'
'Khanna, Shruti'
'Tripathi, Santosh K.'
'Verma, Sandeep'
_publ_section_title
;
 N9 substituent mediated structural tuning of copper--purine complexes:
 chelate effect and thin film studies
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C7CE01017F
_journal_year                    2017
_chemical_formula_sum            'C8 H9 Cl5 Cu2 N4 O'
_chemical_formula_weight         481.52
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2016-10-04 deposited with the CCDC.
2017-07-10 downloaded from the CCDC.
;
_cell_angle_alpha                90.000
_cell_angle_beta                 95.488(5)
_cell_angle_gamma                90.000
_cell_formula_units_Z            4
_cell_length_a                   6.089(4)
_cell_length_b                   14.910(5)
_cell_length_c                   16.172(6)
_cell_measurement_reflns_used    2571
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      4.2
_cell_volume                     1461.5(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker D8 Advance diffractometer'
_diffrn_measurement_method       θ/2θ
_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  0.0430
_diffrn_reflns_av_sigmaI/netI    0.0357
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11425
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         4.24
_exptl_absorpt_coefficient_mu    3.820
_exptl_absorpt_correction_T_max  0.5305
_exptl_absorpt_correction_T_min  0.4870
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North et al., 1968)'
_exptl_crystal_colour            blue-green
_exptl_crystal_density_diffrn    2.188
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block-type
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.534
_refine_diff_density_min         -0.844
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     176
_refine_ls_number_reflns         2571
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0387
_refine_ls_R_factor_gt           0.0276
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0303P)²+1.2635P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0625
_refine_ls_wR_factor_ref         0.0659
_reflns_number_gt                2140
_reflns_number_total             2571
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7ce01017f2.cif
_cod_data_source_block           27augf_0m
_cod_original_cell_volume        1461.5(14)
_cod_database_code               7228799
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, 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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Cu1 Cu 0.82003(6) 0.04146(2) 0.76185(2) 0.00923(12) Uani 1 1 d .
Cl03 Cl 1.12215(13) 0.02260(5) 0.69048(5) 0.01242(18) Uani 1 1 d .
Cl04 Cl 1.03258(13) -0.02302(5) 0.87204(5) 0.01234(19) Uani 1 1 d .
Cl05 Cl 0.59067(13) -0.09906(5) 0.71160(5) 0.01125(18) Uani 1 1 d .
Cl2 Cl 0.56371(13) 0.08270(5) 0.84855(5) 0.01128(18) Uani 1 1 d .
Cl1 Cl 0.89506(13) 0.25418(5) 0.75325(5) 0.01498(19) Uani 1 1 d .
C4 C 0.4444(5) 0.2281(2) 0.56246(19) 0.0088(7) Uani 1 1 d .
C2 C 0.5484(5) 0.0926(2) 0.6049(2) 0.0108(7) Uani 1 1 d .
H2 H 0.5403 0.0306 0.5992 0.013 Uiso 1 1 calc R
C5 C 0.5750(5) 0.2684(2) 0.62693(19) 0.0084(7) Uani 1 1 d .
C6 C 0.7008(5) 0.2125(2) 0.67968(19) 0.0098(7) Uani 1 1 d .
C13 C -0.0845(6) 0.1182(2) 0.4717(2) 0.0181(8) Uani 1 1 d .
H13A H -0.0912 0.0659 0.5060 0.027 Uiso 1 1 calc R
H13B H 0.0417 0.1142 0.4406 0.027 Uiso 1 1 calc R
H13C H -0.2162 0.1219 0.4342 0.027 Uiso 1 1 calc R
C10 C 0.1764(5) 0.2875(2) 0.4451(2) 0.0122(7) Uani 1 1 d .
H10A H 0.2105 0.2364 0.4115 0.015 Uiso 1 1 calc R
H10B H 0.1772 0.3409 0.4108 0.015 Uiso 1 1 calc R
C8 C 1.5871(5) -0.1268(2) 0.9459(2) 0.0104(7) Uani 1 1 d .
H8 H 1.6342 -0.0704 0.9646 0.013 Uiso 1 1 calc R
N7 N 1.4460(4) -0.13961(17) 0.87987(16) 0.0099(6) Uani 1 1 d .
O12 O -0.0662(4) 0.19629(14) 0.52289(13) 0.0125(5) Uani 1 1 d .
N1 N 0.6806(4) 0.12372(17) 0.67086(16) 0.0092(6) Uani 1 1 d .
N9 N 0.3436(4) 0.29598(17) 0.51614(16) 0.0088(6) Uani 1 1 d .
N3 N 0.4298(4) 0.13972(17) 0.54791(16) 0.0098(6) Uani 1 1 d .
C11 C -0.0503(5) 0.2754(2) 0.4754(2) 0.0133(7) Uani 1 1 d .
H11A H -0.0828 0.3268 0.5089 0.016 Uiso 1 1 calc R
H11B H -0.1600 0.2733 0.4278 0.016 Uiso 1 1 calc R
Cu2 Cu 1.32662(6) -0.05211(2) 0.79472(2) 0.00913(12) Uiso 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'
Cl Cl 0.1484 0.1585 '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'
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
N1 Cu1 Cl2 91.11(8) . .
N1 Cu1 Cl03 90.53(8) . .
Cl2 Cu1 Cl03 167.74(3) . .
N1 Cu1 Cl04 166.38(8) . .
Cl2 Cu1 Cl04 90.22(5) . .
Cl03 Cu1 Cl04 85.39(5) . .
N1 Cu1 Cl05 94.87(8) . .
Cl2 Cu1 Cl05 91.76(5) . .
Cl03 Cu1 Cl05 100.21(5) . .
Cl04 Cu1 Cl05 98.63(4) . .
Cu1 Cl03 Cu2 95.48(5) . .
Cu1 Cl04 Cu2 93.80(5) . .
Cu2 Cl05 Cu1 87.52(5) 1_455 .
Cu1 Cl2 Cu2 88.64(5) . 1_455
N3 C4 N9 127.7(3) . .
N3 C4 C5 125.6(3) . .
N9 C4 C5 106.6(3) . .
N3 C2 N1 127.8(3) . .
C6 C5 N7 134.0(3) . 2_756
C6 C5 C4 116.8(3) . .
N7 C5 C4 109.2(3) 2_756 .
N1 C6 C5 119.7(3) . .
N1 C6 Cl1 119.0(2) . .
C5 C6 Cl1 121.3(2) . .
N9 C10 C11 110.0(3) . .
N7 C8 N9 113.3(3) . 2_746
C8 N7 C5 104.8(3) . 2_746
C8 N7 Cu2 129.4(2) . .
C5 N7 Cu2 125.0(2) 2_746 .
C11 O12 C13 111.8(2) . .
C6 N1 C2 117.7(3) . .
C6 N1 Cu1 119.4(2) . .
C2 N1 Cu1 122.5(2) . .
C8 N9 C4 106.1(3) 2_756 .
C8 N9 C10 126.3(3) 2_756 .
C4 N9 C10 127.3(3) . .
C2 N3 C4 112.2(3) . .
O12 C11 C10 112.7(3) . .
N7 Cu2 Cl03 165.79(8) . .
N7 Cu2 Cl05 88.59(8) . 1_655
Cl03 Cu2 Cl05 94.54(5) . 1_655
N7 Cu2 Cl04 89.95(8) . .
Cl03 Cu2 Cl04 84.98(5) . .
Cl05 Cu2 Cl04 171.79(3) 1_655 .
N7 Cu2 Cl2 97.02(8) . 1_655
Cl03 Cu2 Cl2 96.72(4) . 1_655
Cl05 Cu2 Cl2 91.98(5) 1_655 1_655
Cl04 Cu2 Cl2 96.22(5) . 1_655
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 N1 2.037(3) .
Cu1 Cl2 2.2800(13) .
Cu1 Cl03 2.2808(16) .
Cu1 Cl04 2.3095(11) .
Cu1 Cl05 2.6044(12) .
Cl03 Cu2 2.2872(11) .
Cl04 Cu2 2.3207(15) .
Cl05 Cu2 2.3011(13) 1_455
Cl2 Cu2 2.5771(12) 1_455
Cl1 C6 1.712(3) .
C4 N3 1.340(4) .
C4 N9 1.370(4) .
C4 C5 1.386(4) .
C2 N3 1.318(4) .
C2 N1 1.355(4) .
C5 C6 1.373(4) .
C5 N7 1.381(4) 2_756
C6 N1 1.335(4) .
C13 O12 1.427(4) .
C10 N9 1.466(4) .
C10 C11 1.519(4) .
C8 N7 1.319(4) .
C8 N9 1.352(4) 2_746
N7 C5 1.381(4) 2_746
N7 Cu2 1.984(3) .
O12 C11 1.416(4) .
N9 C8 1.352(4) 2_756
Cu2 Cl05 2.3011(13) 1_655
Cu2 Cl2 2.5771(12) 1_655
