#------------------------------------------------------------------------------
#$Date: 2016-03-25 23:43:34 +0100 (vie 25 de mar de 2016) $
#$Revision: 180093 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/39/7053907.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_7053907
loop_
_publ_author_name
'Salmon, Lionel'
'Thuéry, Pierre'
'Rivière, Eric'
'Costes, Jean-Pierre'
'. Mota, Antonio J'
'Ephritikhine, Michel'
_publ_section_title
;
 Structural, magnetic and theoretical calculations of a ferromagnetically
 coupled tetranuclear copper(ii) square complex
;
_journal_issue                   3
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1306
_journal_paper_doi               10.1039/c3nj01512b
_journal_volume                  38
_journal_year                    2014
_chemical_formula_sum            'C58 H64 N4 O11 Zn2'
_chemical_formula_weight         1123.87
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 103.294(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.235(3)
_cell_length_b                   16.9476(18)
_cell_length_c                   13.042(3)
_cell_measurement_reflns_used    16859
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      2.06
_cell_volume                     2631.8(9)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'Kappa-CCD software (Nonius B.V., 1998)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1999)'
_computing_publication_material  'SHELXTL (Sheldrick, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.921
_diffrn_measured_fraction_theta_max 0.921
_diffrn_measurement_device_type  'Nonius Kappa-CCD'
_diffrn_measurement_method       'φ scans'
_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  0.1157
_diffrn_reflns_av_unetI/netI     0.1233
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            16859
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.06
_diffrn_standards_decay_%        none
_diffrn_standards_interval_time  0
_exptl_absorpt_coefficient_mu    0.977
_exptl_absorpt_correction_T_max  0.947
_exptl_absorpt_correction_T_min  0.884
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   'program DELABS from PLATON (Spek, 2000)'
_exptl_crystal_colour            'translucent light yellow'
_exptl_crystal_density_diffrn    1.418
_exptl_crystal_density_meas      ?
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1176
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.756
_refine_diff_density_min         -0.495
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     355
_refine_ls_number_reflns         4594
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.2079
_refine_ls_R_factor_gt           0.0936
_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)+(0.0714P)²+0.9714P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1711
_refine_ls_wR_factor_ref         0.2204
_reflns_number_gt                2167
_reflns_number_total             4594
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3nj01512b.txt
_cod_data_source_block           1.3THF
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7053907
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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
Zn Zn 0.42192(10) 0.53913(6) 0.22204(8) 0.0288(3) Uani 1 1 d .
N1 N 0.3454(6) 0.4602(4) 0.2979(5) 0.0294(17) Uani 1 1 d .
N2 N 0.4540(7) 0.4040(4) 0.6767(5) 0.0291(19) Uani 1 1 d .
O1 O 0.4441(7) 0.3985(4) -0.0736(5) 0.0421(19) Uani 1 1 d .
H1 H 0.4815 0.4420 -0.0360 0.051 Uiso 1 1 d R
O2 O 0.4350(6) 0.4710(3) 0.1068(4) 0.0340(16) Uani 1 1 d .
O3 O 0.6598(6) 0.3688(3) 0.8356(5) 0.0374(17) Uani 1 1 d .
O4 O 0.7650(7) 0.2622(4) 0.9729(6) 0.054(2) Uani 1 1 d .
H4 H 0.8031 0.3052 0.9453 0.064 Uiso 1 1 d R
C1 C 0.3874(9) 0.3638(5) -0.0077(7) 0.031(2) Uani 1 1 d .
C2 C 0.3790(9) 0.4014(5) 0.0874(7) 0.031(2) Uani 1 1 d .
C3 C 0.3183(8) 0.3635(5) 0.1514(6) 0.027(2) Uani 1 1 d .
C4 C 0.2661(9) 0.2915(5) 0.1210(7) 0.036(3) Uani 1 1 d .
H4A H 0.2261 0.2669 0.1647 0.043 Uiso 1 1 calc R
C5 C 0.2725(10) 0.2562(5) 0.0284(8) 0.046(3) Uani 1 1 d .
H5 H 0.2376 0.2079 0.0093 0.055 Uiso 1 1 calc R
C6 C 0.3311(10) 0.2928(5) -0.0363(7) 0.041(3) Uani 1 1 d .
H6 H 0.3332 0.2697 -0.1005 0.050 Uiso 1 1 calc R
C7 C 0.3079(9) 0.3925(5) 0.2514(7) 0.038(3) Uani 1 1 d .
H7 H 0.2699 0.3599 0.2888 0.046 Uiso 1 1 calc R
C8 C 0.3287(8) 0.4709(5) 0.4037(6) 0.030(2) Uani 1 1 d .
C9 C 0.4011(9) 0.4310(5) 0.4884(6) 0.027(2) Uani 1 1 d .
C10 C 0.3841(8) 0.4441(4) 0.5873(7) 0.025(2) Uani 1 1 d .
C11 C 0.3044(8) 0.4962(5) 0.6093(7) 0.027(2) Uani 1 1 d .
C12 C 0.2366(8) 0.5355(5) 0.5209(6) 0.029(2) Uani 1 1 d .
H12 H 0.1828 0.5710 0.5325 0.034 Uiso 1 1 calc R
C13 C 0.2466(8) 0.5239(4) 0.4199(7) 0.030(2) Uani 1 1 d .
C14 C 0.4876(9) 0.3746(5) 0.4684(6) 0.030(2) Uani 1 1 d .
H14A H 0.5489 0.3723 0.5294 0.045 Uiso 1 1 calc R
H14B H 0.5147 0.3922 0.4088 0.045 Uiso 1 1 calc R
H14C H 0.4548 0.3232 0.4543 0.045 Uiso 1 1 calc R
C15 C 0.2876(9) 0.5101(6) 0.7188(7) 0.039(3) Uani 1 1 d .
H15A H 0.3538 0.5340 0.7614 0.058 Uiso 1 1 calc R
H15B H 0.2739 0.4606 0.7495 0.058 Uiso 1 1 calc R
H15C H 0.2245 0.5444 0.7153 0.058 Uiso 1 1 calc R
C16 C 0.1694(10) 0.5643(6) 0.3271(7) 0.043(3) Uani 1 1 d .
H16A H 0.1198 0.5994 0.3522 0.064 Uiso 1 1 calc R
H16B H 0.1261 0.5253 0.2819 0.064 Uiso 1 1 calc R
H16C H 0.2135 0.5938 0.2883 0.064 Uiso 1 1 calc R
C17 C 0.4431(9) 0.3281(5) 0.6850(7) 0.032(2) Uani 1 1 d .
H17 H 0.3852 0.3044 0.6358 0.039 Uiso 1 1 calc R
C18 C 0.5110(9) 0.2765(5) 0.7622(7) 0.032(2) Uani 1 1 d .
C19 C 0.6106(10) 0.2992(5) 0.8324(7) 0.040(3) Uani 1 1 d .
C20 C 0.6684(10) 0.2401(6) 0.9079(7) 0.039(3) Uani 1 1 d .
C21 C 0.6246(11) 0.1678(6) 0.9112(9) 0.051(3) Uani 1 1 d .
H21 H 0.6594 0.1323 0.9628 0.062 Uiso 1 1 calc R
C22 C 0.5256(11) 0.1449(5) 0.8369(9) 0.047(3) Uani 1 1 d .
H22 H 0.4983 0.0939 0.8396 0.056 Uiso 1 1 calc R
C23 C 0.4680(10) 0.1969(5) 0.7597(9) 0.041(3) Uani 1 1 d .
H23 H 0.4051 0.1809 0.7093 0.050 Uiso 1 1 calc R
O5 O 0.4049(12) 0.7043(8) 0.7360(10) 0.135(5) Uani 1 1 d U
C24 C 0.3582(14) 0.7223(8) 0.8325(12) 0.087(5) Uani 1 1 d U
H24A H 0.2842 0.6997 0.8268 0.104 Uiso 1 1 calc R
H24B H 0.4083 0.7047 0.8974 0.104 Uiso 1 1 calc R
C25 C 0.3547(18) 0.8064(10) 0.8239(15) 0.119(6) Uani 1 1 d U
H25A H 0.2768 0.8219 0.8151 0.143 Uiso 1 1 calc R
H25B H 0.3948 0.8271 0.8915 0.143 Uiso 1 1 calc R
C26 C 0.3970(15) 0.8471(9) 0.7444(13) 0.099(5) Uani 1 1 d U
H26A H 0.4497 0.8883 0.7744 0.119 Uiso 1 1 calc R
H26B H 0.3368 0.8695 0.6906 0.119 Uiso 1 1 calc R
C27 C 0.4529(13) 0.7812(8) 0.7030(11) 0.079(4) Uani 1 1 d U
H27A H 0.5334 0.7834 0.7316 0.095 Uiso 1 1 calc R
H27B H 0.4389 0.7844 0.6268 0.095 Uiso 1 1 calc R
O6 O 0.886(2) 0.4031(11) 1.0219(16) 0.093(6) Uani 0.50 1 d PU
C28 C 0.9564(18) 0.5316(11) 1.0042(16) 0.127(7) Uani 1 1 d U
C29 C 0.858(3) 0.4857(18) 1.002(3) 0.098(11) Uani 0.50 1 d PU
C30 C 1.000(4) 0.394(2) 1.021(3) 0.131(14) Uani 0.50 1 d PU
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'
Zn Zn 0.2839 1.4301 '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
O3 Zn O2 108.2(3) 3_666 .
O3 Zn N2 96.6(3) 3_666 3_666
O2 Zn N2 127.7(3) . 3_666
O3 Zn N1 118.3(3) 3_666 .
O2 Zn N1 96.7(3) . .
N2 Zn N1 111.1(3) 3_666 .
O3 Zn Zn 122.78(19) 3_666 3_666
O2 Zn Zn 128.66(18) . 3_666
N2 Zn Zn 56.0(2) 3_666 3_666
N1 Zn Zn 55.1(2) . 3_666
C7 N1 C8 115.7(8) . .
C7 N1 Zn 119.9(6) . .
C8 N1 Zn 124.4(6) . .
C17 N2 C10 118.6(8) . .
C17 N2 Zn 119.6(7) . 3_666
C10 N2 Zn 121.4(5) . 3_666
C2 O2 Zn 122.4(5) . .
C19 O3 Zn 121.5(7) . 3_666
O1 C1 C6 119.9(8) . .
O1 C1 C2 120.6(8) . .
C6 C1 C2 119.4(9) . .
O2 C2 C3 127.2(8) . .
O2 C2 C1 114.8(8) . .
C3 C2 C1 118.0(9) . .
C4 C3 C2 120.5(8) . .
C4 C3 C7 115.5(8) . .
C2 C3 C7 124.0(9) . .
C5 C4 C3 121.3(9) . .
C4 C5 C6 119.3(9) . .
C5 C6 C1 121.4(9) . .
N1 C7 C3 128.4(9) . .
C13 C8 C9 122.0(8) . .
C13 C8 N1 119.1(8) . .
C9 C8 N1 118.8(8) . .
C10 C9 C8 116.9(8) . .
C10 C9 C14 122.3(7) . .
C8 C9 C14 120.7(7) . .
C9 C10 C11 124.1(8) . .
C9 C10 N2 119.5(8) . .
C11 C10 N2 116.4(7) . .
C10 C11 C12 115.9(8) . .
C10 C11 C15 123.2(8) . .
C12 C11 C15 120.9(8) . .
C13 C12 C11 123.3(8) . .
C12 C13 C8 117.8(8) . .
C12 C13 C16 121.9(8) . .
C8 C13 C16 120.4(8) . .
N2 C17 C18 127.2(9) . .
C19 C18 C17 124.4(8) . .
C19 C18 C23 121.9(8) . .
C17 C18 C23 113.7(9) . .
O3 C19 C18 126.0(8) . .
O3 C19 C20 116.2(10) . .
C18 C19 C20 117.7(9) . .
O4 C20 C21 122.4(10) . .
O4 C20 C19 117.0(9) . .
C21 C20 C19 120.7(11) . .
C20 C21 C22 120.8(10) . .
C23 C22 C21 121.9(9) . .
C22 C23 C18 116.8(10) . .
C24 O5 C27 107.5(11) . .
C25 C24 O5 98.3(13) . .
C26 C25 C24 121.7(16) . .
C25 C26 C27 100.1(14) . .
C26 C27 O5 107.5(13) . .
C30 O6 C29 107(3) . .
C29 C28 C28 102(2) . 3_767
C30 C28 C28 107(3) 3_767 3_767
C28 C29 O6 111(3) . .
O6 C30 C28 110(3) . 3_767
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn O3 1.912(6) 3_666
Zn O2 1.930(6) .
Zn N2 2.014(7) 3_666
Zn N1 2.018(8) .
Zn Zn 7.183(3) 3_666
N1 C7 1.328(11) .
N1 C8 1.451(10) .
N2 C17 1.301(10) .
N2 C10 1.446(11) .
N2 Zn 2.014(7) 3_666
O1 C1 1.356(11) .
O2 C2 1.358(11) .
O3 C19 1.320(11) .
O3 Zn 1.912(6) 3_666
O4 C20 1.339(13) .
C1 C6 1.394(12) .
C1 C2 1.419(12) .
C2 C3 1.396(13) .
C3 C4 1.392(12) .
C3 C7 1.427(12) .
C4 C5 1.367(13) .
C5 C6 1.374(14) .
C8 C13 1.399(12) .
C8 C9 1.419(12) .
C9 C10 1.372(11) .
C9 C14 1.492(13) .
C10 C11 1.393(12) .
C11 C12 1.422(12) .
C11 C15 1.508(11) .
C12 C13 1.364(11) .
C13 C16 1.517(12) .
C17 C18 1.443(13) .
C18 C19 1.399(14) .
C18 C23 1.447(12) .
C19 C20 1.467(13) .
C20 C21 1.342(14) .
C21 C22 1.420(16) .
C22 C23 1.400(14) .
O5 C24 1.528(18) .
O5 C27 1.532(17) .
C24 C25 1.429(19) .
C25 C26 1.44(2) .
C26 C27 1.475(19) .
O6 C30 1.40(5) .
O6 C29 1.45(3) .
C28 C29 1.43(4) .
C28 C30 1.43(4) 3_767
C28 C28 1.53(4) 3_767
C30 C28 1.43(4) 3_767
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1 O2 0.94 2.13 2.680(8) 116.1 .
O1 H1 O2 0.94 2.12 2.751(9) 122.8 3_665
O4 H4 O3 0.98 2.26 2.658(9) 102.8 .
O4 H4 O6 0.98 2.08 2.81(2) 129.8 .
