#------------------------------------------------------------------------------
#$Date: 2016-03-25 09:36:42 +0100 (vie 25 de mar de 2016) $
#$Revision: 179756 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/52/7005285.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_7005285
loop_
_publ_author_name
'Sílvia Carvalho'
'Rita Delgado'
'Michael G. B. Drew'
'Vítor Félix'
_publ_section_title
;
 Dicopper(ii) complexes of a new di-para-xylyldioxatetraazamacrocycle
 and cascade species with dicarboxylate anions: thermodynamics and
 structural properties
;
_journal_issue                   23
_journal_name_full               'Dalton Transactions'
_journal_page_first              2431
_journal_paper_doi               10.1039/b700115k
_journal_year                    2007
_chemical_formula_sum            'C30 H46 Cu2 N4 O18'
_chemical_formula_weight         877.80
_chemical_name_systematic
;
?
;
_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                 110.180(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.211(15)
_cell_length_b                   12.976(17)
_cell_length_c                   13.812(18)
_cell_measurement_temperature    293(2)
_cell_volume                     1886(4)
_computing_cell_refinement       XDS
_computing_data_collection       'XDS (Kabsch, 1991)'
_computing_data_reduction        XDS
_computing_molecular_graphics    'PLATON (Speck, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.929
_diffrn_measured_fraction_theta_max 0.929
_diffrn_measurement_device_type  'Mar-research Image Plate'
_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  0.1075
_diffrn_reflns_av_sigmaI/netI    0.1083
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10199
_diffrn_reflns_theta_full        25.80
_diffrn_reflns_theta_max         25.80
_diffrn_reflns_theta_min         2.22
_exptl_absorpt_coefficient_mu    1.209
_exptl_absorpt_correction_T_max  0.786
_exptl_absorpt_correction_T_min  0.704
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.542
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelopiped
_exptl_crystal_F_000             908
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.747
_refine_diff_density_min         -0.538
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     256
_refine_ls_number_reflns         3369
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.1446
_refine_ls_R_factor_gt           0.0995
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0308P)²+12.3843P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1757
_refine_ls_wR_factor_ref         0.1923
_reflns_number_gt                2145
_reflns_number_total             3369
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b700115k.txt
_cod_data_source_block           compound1
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Empirical' changed to
'empirical' 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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0308P)^2^+12.3843P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0308P)^2^+12.3843P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7005285
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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu Cu 0.48847(10) 0.87089(9) 0.15372(7) 0.0432(3) Uani 1 d . . .
C11 C 0.8736(10) 0.7648(8) 0.0926(9) 0.071(3) Uani 1 d . . .
H11A H 0.9130 0.7182 0.0577 0.085 Uiso 1 calc R . .
H11B H 0.9298 0.7720 0.1636 0.085 Uiso 1 calc R . .
N12 N 0.7465(8) 0.7221(6) 0.0893(7) 0.056(2) Uani 1 d D . .
H12 H 0.717(9) 0.763(6) 0.118(7) 0.067 Uiso 1 d D . .
C13 C 0.7555(12) 0.6231(8) 0.1469(11) 0.094(4) Uani 1 d . . .
H13A H 0.8065 0.5743 0.1249 0.113 Uiso 1 calc R . .
H13B H 0.7972 0.6353 0.2201 0.113 Uiso 1 calc R . .
C14 C 0.6273(12) 0.5785(8) 0.1284(11) 0.086(4) Uani 1 d . . .
H14A H 0.5857 0.5653 0.0553 0.104 Uiso 1 calc R . .
H14B H 0.6355 0.5135 0.1648 0.104 Uiso 1 calc R . .
O15 O 0.5526(6) 0.6479(4) 0.1632(5) 0.0494(16) Uani 1 d . . .
C16 C 0.4253(9) 0.6077(6) 0.1364(7) 0.052(2) Uani 1 d . . .
H16A H 0.4268 0.5427 0.1714 0.062 Uiso 1 calc R . .
H16B H 0.3895 0.5959 0.0626 0.062 Uiso 1 calc R . .
C17 C 0.3469(9) 0.6838(7) 0.1680(7) 0.052(2) Uani 1 d . . .
H17A H 0.3867 0.6977 0.2411 0.062 Uiso 1 calc R . .
H17B H 0.2640 0.6539 0.1574 0.062 Uiso 1 calc R . .
N18 N 0.3293(7) 0.7840(6) 0.1099(5) 0.0389(17) Uani 1 d D . .
H18 H 0.302(7) 0.768(6) 0.0504(19) 0.047 Uiso 1 d D . .
C19 C 0.2143(9) 0.8381(7) 0.1169(7) 0.048(2) Uani 1 d . . .
H19A H 0.2249 0.8485 0.1889 0.058 Uiso 1 calc R . .
H19B H 0.1402 0.7947 0.0866 0.058 Uiso 1 calc R . .
C20 C 0.1920(7) 0.9406(7) 0.0627(6) 0.038(2) Uani 1 d . . .
C21 C 0.1959(10) 1.0292(8) 0.1158(8) 0.064(3) Uani 1 d . . .
H21 H 0.2139 1.0268 0.1867 0.077 Uiso 1 calc R . .
C22 C 0.1733(11) 1.1233(9) 0.0656(9) 0.074(3) Uani 1 d . . .
H22 H 0.1751 1.1829 0.1034 0.089 Uiso 1 calc R . .
C23 C 0.1480(9) 1.1309(9) -0.0398(8) 0.058(3) Uani 1 d . . .
C24 C 0.1434(10) 1.0416(9) -0.0936(8) 0.064(3) Uani 1 d . . .
H24 H 0.1263 1.0443 -0.1644 0.077 Uiso 1 calc R . .
C25 C 0.1641(9) 0.9471(8) -0.0435(7) 0.060(3) Uani 1 d . . .
H25 H 0.1592 0.8870 -0.0814 0.072 Uiso 1 calc R . .
O41 O 0.5055(6) 0.8659(5) 0.0180(4) 0.0459(14) Uani 1 d . . .
O42 O 0.5104(5) 0.9597(4) -0.1174(4) 0.0430(15) Uani 1 d . . .
C43 C 0.5044(7) 0.9505(6) -0.0292(6) 0.0347(19) Uani 1 d . . .
O51 O 0.4854(6) 0.8811(6) 0.2936(4) 0.0621(19) Uani 1 d . . .
C52 C 0.5918(10) 0.8608(8) 0.3640(7) 0.055(2) Uani 1 d . . .
O53 O 0.6071(8) 0.8566(7) 0.4565(5) 0.092(3) Uani 1 d . . .
C54 C 0.7026(9) 0.8402(6) 0.3257(7) 0.046(2) Uani 1 d . . .
O55 O 0.6784(5) 0.8578(5) 0.2297(4) 0.0471(15) Uani 1 d . . .
O56 O 0.8047(7) 0.8090(6) 0.3873(5) 0.075(2) Uani 1 d . . .
O100 O 0.5474(10) 0.7238(8) -0.1361(7) 0.125(4) Uani 1 d . . .
O200 O 0.3226(13) 0.9515(17) 0.4127(10) 0.215(8) Uani 1 d D . .
H201 H 0.371(9) 0.95(2) 0.473(3) 0.258 Uiso 1 d D . .
H202 H 0.369(10) 0.94(2) 0.380(8) 0.258 Uiso 1 d 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'
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
O51 Cu O41 175.3(3) . . ?
O51 Cu N18 91.1(3) . . ?
O41 Cu N18 93.6(3) . . ?
O51 Cu O55 82.4(3) . . ?
O41 Cu O55 93.5(2) . . ?
N18 Cu O55 140.3(3) . . ?
O51 Cu O42 99.1(3) . 3_675 ?
O41 Cu O42 79.0(2) . 3_675 ?
N18 Cu O42 123.3(3) . 3_675 ?
O55 Cu O42 96.4(2) . 3_675 ?
N12 C11 C23 108.6(8) . 3_675 ?
N12 C11 H11A 110.0 . . ?
C23 C11 H11A 110.0 3_675 . ?
N12 C11 H11B 110.0 . . ?
C23 C11 H11B 110.0 3_675 . ?
H11A C11 H11B 108.3 . . ?
C13 N12 C11 114.1(8) . . ?
C13 N12 H12 106(7) . . ?
C11 N12 H12 107(7) . . ?
C14 C13 N12 111.1(10) . . ?
C14 C13 H13A 109.4 . . ?
N12 C13 H13A 109.4 . . ?
C14 C13 H13B 109.4 . . ?
N12 C13 H13B 109.4 . . ?
H13A C13 H13B 108.0 . . ?
O15 C14 C13 110.0(9) . . ?
O15 C14 H14A 109.7 . . ?
C13 C14 H14A 109.7 . . ?
O15 C14 H14B 109.7 . . ?
C13 C14 H14B 109.7 . . ?
H14A C14 H14B 108.2 . . ?
C14 O15 C16 109.3(7) . . ?
O15 C16 C17 108.6(7) . . ?
O15 C16 H16A 110.0 . . ?
C17 C16 H16A 110.0 . . ?
O15 C16 H16B 110.0 . . ?
C17 C16 H16B 110.0 . . ?
H16A C16 H16B 108.4 . . ?
C16 C17 N18 113.5(7) . . ?
C16 C17 H17A 108.9 . . ?
N18 C17 H17A 108.9 . . ?
C16 C17 H17B 108.9 . . ?
N18 C17 H17B 108.9 . . ?
H17A C17 H17B 107.7 . . ?
C19 N18 C17 109.1(6) . . ?
C19 N18 Cu 114.2(6) . . ?
C17 N18 Cu 112.5(5) . . ?
C19 N18 H18 99(6) . . ?
C17 N18 H18 105(6) . . ?
Cu N18 H18 116(6) . . ?
N18 C19 C20 112.4(7) . . ?
N18 C19 H19A 109.1 . . ?
C20 C19 H19A 109.1 . . ?
N18 C19 H19B 109.1 . . ?
C20 C19 H19B 109.1 . . ?
H19A C19 H19B 107.9 . . ?
C21 C20 C25 118.2(9) . . ?
C21 C20 C19 120.8(8) . . ?
C25 C20 C19 121.0(8) . . ?
C20 C21 C22 120.7(9) . . ?
C20 C21 H21 119.6 . . ?
C22 C21 H21 119.6 . . ?
C21 C22 C23 121.6(11) . . ?
C21 C22 H22 119.2 . . ?
C23 C22 H22 119.2 . . ?
C24 C23 C22 117.8(10) . . ?
C24 C23 C11 121.6(9) . 3_675 ?
C22 C23 C11 120.6(11) . 3_675 ?
C23 C24 C25 120.6(9) . . ?
C23 C24 H24 119.7 . . ?
C25 C24 H24 119.7 . . ?
C24 C25 C20 121.1(10) . . ?
C24 C25 H25 119.4 . . ?
C20 C25 H25 119.4 . . ?
C43 O41 Cu 118.4(5) . . ?
C43 O42 Cu 108.5(5) . 3_675 ?
O42 C43 O41 125.9(7) . . ?
O42 C43 C43 117.8(9) . 3_675 ?
O41 C43 C43 116.3(8) . 3_675 ?
C52 O51 Cu 114.1(6) . . ?
O53 C52 O51 123.9(9) . . ?
O53 C52 C54 120.8(9) . . ?
O51 C52 C54 115.4(8) . . ?
O56 C54 O55 126.0(9) . . ?
O56 C54 C52 119.2(8) . . ?
O55 C54 C52 114.8(8) . . ?
C54 O55 Cu 111.1(6) . . ?
H201 O200 H202 103.7(3) . . ?
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
Cu O51 1.949(6) . ?
Cu O41 1.950(6) . ?
Cu N18 2.019(7) . ?
Cu O55 2.030(6) . ?
Cu O42 2.256(6) 3_675 ?
C11 N12 1.515(12) . ?
C11 C23 1.517(13) 3_675 ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
N12 C13 1.496(12) . ?
N12 H12 0.8000(12) . ?
C13 C14 1.487(15) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 O15 1.421(11) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
O15 C16 1.443(10) . ?
C16 C17 1.485(12) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 N18 1.504(10) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
N18 C19 1.500(11) . ?
N18 H18 0.8000(14) . ?
C19 C20 1.505(11) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 C21 1.357(12) . ?
C20 C25 1.392(12) . ?
C21 C22 1.383(14) . ?
C21 H21 0.9300 . ?
C22 C23 1.386(14) . ?
C22 H22 0.9300 . ?
C23 C24 1.367(14) . ?
C23 C11 1.517(13) 3_675 ?
C24 C25 1.389(13) . ?
C24 H24 0.9300 . ?
C25 H25 0.9300 . ?
O41 C43 1.275(9) . ?
O42 C43 1.249(8) . ?
O42 Cu 2.256(6) 3_675 ?
C43 C43 1.538(16) 3_675 ?
O51 C52 1.279(10) . ?
C52 O53 1.231(10) . ?
C52 C54 1.533(13) . ?
C54 O56 1.235(10) . ?
C54 O55 1.279(10) . ?
O200 H201 0.8200(18) . ?
O200 H202 0.820(2) . ?
