#------------------------------------------------------------------------------
#$Date: 2016-03-26 17:00:14 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180367 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/36/7203641.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_7203641
loop_
_publ_author_name
'Doyle, Robert P.'
'Nieuwenhuyzen, Mark'
'Kruger, Paul E.'
_publ_section_title
;
 A molecular ?back-flip?: the structural consequences of the
 crystal-to-crystal phase transition between [(phen)2CuCO3]?11H2O and
 [(phen)2CuCO3]?7H2O
;
_journal_issue                   12
_journal_name_full               CrystEngComm
_journal_page_first              904
_journal_paper_doi               10.1039/b612319h
_journal_volume                  8
_journal_year                    2006
_chemical_formula_sum            'C25 H38 Cu N4 O14'
_chemical_formula_weight         682.13
_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
_cell_angle_alpha                77.732(9)
_cell_angle_beta                 77.628(5)
_cell_angle_gamma                70.025(5)
_cell_formula_units_Z            2
_cell_length_a                   10.873(2)
_cell_length_b                   11.598(2)
_cell_length_c                   13.394(3)
_cell_measurement_temperature    153(2)
_cell_volume                     1532.6(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.864
_diffrn_measured_fraction_theta_max 0.864
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0375
_diffrn_reflns_av_sigmaI/netI    0.0579
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14146
_diffrn_reflns_theta_full        28.42
_diffrn_reflns_theta_max         28.42
_diffrn_reflns_theta_min         1.57
_exptl_absorpt_coefficient_mu    0.786
_exptl_absorpt_correction_T_max  0.9116
_exptl_absorpt_correction_T_min  0.7137
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.478
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       diamond-block
_exptl_crystal_F_000             714
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.880
_refine_diff_density_min         -0.913
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     427
_refine_ls_number_reflns         6678
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0919
_refine_ls_R_factor_gt           0.0625
_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)+(0.0979P)²+0.2903P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1659
_refine_ls_wR_factor_ref         0.1844
_reflns_number_gt                4529
_reflns_number_total             6678
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b612319h.txt
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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:

'_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_cell_volume        1532.7(6)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7203641
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 0.90046(5) -0.76499(4) -0.74889(3) 0.04145(18) Uani 1 1 d . . .
C1 C 0.7505(5) -0.5490(3) -0.6954(4) 0.0667(15) Uani 1 1 d . . .
O13 O 0.6584(5) -0.4489(3) -0.6817(4) 0.124(2) Uani 1 1 d . . .
O12 O 0.8548(3) -0.5867(2) -0.6526(2) 0.0610(9) Uani 1 1 d . . .
O11 O 0.7429(3) -0.6176(2) -0.7583(2) 0.0511(7) Uani 1 1 d . . .
N1A N 1.0180(4) -0.6869(3) -0.8581(2) 0.0471(8) Uani 1 1 d . . .
C2A C 1.0900(5) -0.6214(4) -0.8422(3) 0.0541(11) Uani 1 1 d . . .
H2AA H 1.0841 -0.6074 -0.7737 0.065 Uiso 1 1 calc R . .
C3A C 1.1731(5) -0.5726(4) -0.9207(3) 0.0593(12) Uani 1 1 d . . .
H3AA H 1.2227 -0.5268 -0.9057 0.071 Uiso 1 1 calc R . .
C4A C 1.1827(6) -0.5915(4) -1.0203(3) 0.0600(12) Uani 1 1 d . . .
H4AA H 1.2378 -0.5574 -1.0751 0.072 Uiso 1 1 calc R . .
C5A C 1.1105(5) -0.6615(3) -1.0406(3) 0.0507(11) Uani 1 1 d . . .
C6A C 1.1128(6) -0.6847(4) -1.1429(3) 0.0613(13) Uani 1 1 d . . .
H6AA H 1.1655 -0.6514 -1.2002 0.074 Uiso 1 1 calc R . .
C7A C 1.0432(5) -0.7512(4) -1.1587(3) 0.0623(14) Uani 1 1 d . . .
H7AA H 1.0487 -0.7662 -1.2268 0.075 Uiso 1 1 calc R . .
C8A C 0.9605(4) -0.8009(3) -1.0763(3) 0.0493(11) Uani 1 1 d . . .
C9A C 0.8837(5) -0.8719(4) -1.0878(4) 0.0571(12) Uani 1 1 d . . .
H9AA H 0.8827 -0.8864 -1.1548 0.069 Uiso 1 1 calc R . .
C10A C 0.8109(4) -0.9203(4) -1.0041(4) 0.0560(12) Uani 1 1 d . . .
H10A H 0.7600 -0.9690 -1.0122 0.067 Uiso 1 1 calc R . .
C11A C 0.8122(4) -0.8971(4) -0.9052(4) 0.0500(11) Uani 1 1 d . . .
H11A H 0.7618 -0.9314 -0.8469 0.060 Uiso 1 1 calc R . .
N12A N 0.8814(3) -0.8288(3) -0.8907(3) 0.0438(8) Uani 1 1 d . . .
C13A C 0.9536(4) -0.7809(3) -0.9740(3) 0.0423(9) Uani 1 1 d . . .
C14A C 1.0307(4) -0.7080(3) -0.9575(3) 0.0454(10) Uani 1 1 d . . .
N1B N 0.8014(3) -0.8596(3) -0.6377(2) 0.0382(7) Uani 1 1 d . . .
C2B C 0.6737(4) -0.8268(4) -0.5974(3) 0.0463(10) Uani 1 1 d . . .
H2BA H 0.6187 -0.7463 -0.6210 0.056 Uiso 1 1 calc R . .
C3B C 0.6169(4) -0.9046(4) -0.5224(3) 0.0508(10) Uani 1 1 d . . .
H3BA H 0.5255 -0.8770 -0.4946 0.061 Uiso 1 1 calc R . .
C4B C 0.6950(4) -1.0225(4) -0.4891(3) 0.0461(9) Uani 1 1 d . . .
H4BA H 0.6575 -1.0773 -0.4387 0.055 Uiso 1 1 calc R . .
C5B C 0.8300(4) -1.0612(3) -0.5298(3) 0.0382(8) Uani 1 1 d . . .
C6B C 0.9217(4) -1.1817(3) -0.4987(3) 0.0420(9) Uani 1 1 d . . .
H6BA H 0.8902 -1.2404 -0.4483 0.050 Uiso 1 1 calc R . .
C7B C 1.0521(4) -1.2121(3) -0.5404(3) 0.0418(9) Uani 1 1 d . . .
H7BA H 1.1101 -1.2922 -0.5195 0.050 Uiso 1 1 calc R . .
C8B C 1.1029(4) -1.1253(3) -0.6151(3) 0.0371(8) Uani 1 1 d . . .
C9B C 1.2369(4) -1.1499(4) -0.6611(3) 0.0444(9) Uani 1 1 d . . .
H9BA H 1.2991 -1.2288 -0.6439 0.053 Uiso 1 1 calc R . .
C10B C 1.2770(4) -1.0604(4) -0.7303(3) 0.0467(10) Uani 1 1 d . . .
H10B H 1.3670 -1.0760 -0.7615 0.056 Uiso 1 1 calc R . .
C11B C 1.1831(4) -0.9448(4) -0.7547(3) 0.0452(9) Uani 1 1 d . . .
H11B H 1.2124 -0.8827 -0.8024 0.054 Uiso 1 1 calc R . .
N12B N 1.0567(3) -0.9175(3) -0.7153(2) 0.0381(7) Uani 1 1 d . . .
C13B C 1.0169(4) -1.0077(3) -0.6459(3) 0.0357(8) Uani 1 1 d . . .
C14B C 0.8788(4) -0.9762(3) -0.6033(3) 0.0357(8) Uani 1 1 d . . .
O1W O 0.4267(3) -0.3753(2) -0.11974(19) 0.0427(6) Uani 1 1 d . . .
H1W1 H 0.3804 -0.3950 -0.1517 0.051 Uiso 1 1 d R . .
H1W2 H 0.4563 -0.3160 -0.1504 0.051 Uiso 1 1 d R . .
O2W O 0.0319(3) -0.5552(3) -0.4022(2) 0.0533(7) Uani 1 1 d . . .
H2W2 H 0.0574 -0.4954 -0.3758 0.064 Uiso 1 1 d R . .
H2W1 H 0.0006 -0.5219 -0.4690 0.064 Uiso 1 1 d R . .
O3W O 0.3789(3) -0.3963(3) 0.0994(2) 0.0623(9) Uani 1 1 d . . .
H3W1 H 0.4403 -0.4729 0.1091 0.075 Uiso 1 1 d R . .
H3W2 H 0.3883 -0.3621 0.0333 0.075 Uiso 1 1 d R . .
O4W O 0.2929(3) -0.7224(3) -0.4061(2) 0.0650(9) Uani 1 1 d . . .
H4W1 H 0.3027 -0.6623 -0.3786 0.078 Uiso 1 1 d R . .
H4W2 H 0.2036 -0.6812 -0.4040 0.078 Uiso 1 1 d R . .
O5W O 0.4649(4) -0.8186(4) 0.2149(4) 0.1089(17) Uani 1 1 d . . .
H5W1 H 0.4253 -0.7671 0.2538 0.131 Uiso 1 1 d R . .
H5W2 H 0.5007 -0.8943 0.2449 0.131 Uiso 1 1 d R . .
O6W O 0.3818(4) -0.9339(4) -0.2534(3) 0.0971(14) Uani 1 1 d . . .
H6W2 H 0.3422 -0.8566 -0.3030 0.117 Uiso 1 1 d R . .
H6W1 H 0.3341 -0.9637 -0.2641 0.117 Uiso 1 1 d R . .
O7W O 0.2118(4) -0.4327(4) 0.2861(3) 0.0753(10) Uani 1 1 d . . .
H7W1 H 0.2891 -0.4632 0.3221 0.090 Uiso 1 1 d R . .
H7W2 H 0.1947 -0.4444 0.2206 0.090 Uiso 1 1 d R . .
O8W O 0.4683(4) -0.7240(3) -0.1656(3) 0.0944(14) Uani 1 1 d . . .
H8W1 H 0.5026 -0.7026 -0.1323 0.113 Uiso 1 1 d R . .
H8W2 H 0.4309 -0.6640 -0.2144 0.113 Uiso 1 1 d R . .
O9W O 0.3938(6) -0.8862(5) 0.0344(5) 0.061(2) Uani 0.538(8) 1 d P A 2
O10W O 0.3176(7) -0.7026(6) -0.6323(5) 0.100(3) Uani 0.719(12) 1 d P B 2
O11W O 0.3788(17) -0.4571(8) -0.5792(8) 0.075(4) Uani 0.57(3) 1 d P C 2
O9' O 0.4035(7) -0.9113(6) -0.0639(6) 0.062(3) Uani 0.462(8) 1 d P A 1
O10' O 0.3637(12) -0.6288(14) -0.6098(9) 0.064(5) Uani 0.281(12) 1 d P B 1
O11' O 0.457(2) -0.4485(9) -0.5906(8) 0.075(5) Uani 0.43(3) 1 d P C 1
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
O11 Cu1 N1B 92.22(13) . . ?
O11 Cu1 N1A 94.26(13) . . ?
N1B Cu1 N1A 173.51(12) . . ?
O11 Cu1 N12B 171.21(12) . . ?
N1B Cu1 N12B 81.96(13) . . ?
N1A Cu1 N12B 91.56(13) . . ?
O11 Cu1 N12A 94.21(10) . . ?
N1B Cu1 N12A 101.04(12) . . ?
N1A Cu1 N12A 78.93(12) . . ?
N12B Cu1 N12A 93.37(11) . . ?
O13 C1 O12 123.4(3) . . ?
O13 C1 O11 119.6(4) . . ?
O12 C1 O11 117.0(4) . . ?
C1 O11 Cu1 105.0(2) . . ?
C2A N1A C14A 117.0(4) . . ?
C2A N1A Cu1 125.9(3) . . ?
C14A N1A Cu1 117.0(3) . . ?
N1A C2A C3A 123.3(4) . . ?
C4A C3A C2A 119.3(4) . . ?
C3A C4A C5A 119.5(4) . . ?
C14A C5A C4A 117.6(4) . . ?
C14A C5A C6A 118.9(4) . . ?
C4A C5A C6A 123.4(4) . . ?
C7A C6A C5A 121.5(5) . . ?
C6A C7A C8A 121.6(4) . . ?
C9A C8A C13A 116.0(4) . . ?
C9A C8A C7A 124.4(4) . . ?
C13A C8A C7A 119.6(4) . . ?
C10A C9A C8A 120.8(4) . . ?
C9A C10A C11A 119.0(4) . . ?
N12A C11A C10A 122.3(5) . . ?
C11A N12A C13A 118.5(3) . . ?
C11A N12A Cu1 132.5(3) . . ?
C13A N12A Cu1 109.0(2) . . ?
N12A C13A C8A 123.4(4) . . ?
N12A C13A C14A 118.2(3) . . ?
C8A C13A C14A 118.3(4) . . ?
N1A C14A C5A 123.3(4) . . ?
N1A C14A C13A 116.7(4) . . ?
C5A C14A C13A 120.0(3) . . ?
C2B N1B C14B 117.5(3) . . ?
C2B N1B Cu1 129.4(3) . . ?
C14B N1B Cu1 113.1(3) . . ?
N1B C2B C3B 123.1(4) . . ?
C4B C3B C2B 119.0(4) . . ?
C3B C4B C5B 119.8(4) . . ?
C14B C5B C4B 117.2(3) . . ?
C14B C5B C6B 118.3(4) . . ?
C4B C5B C6B 124.4(4) . . ?
C7B C6B C5B 121.2(4) . . ?
C6B C7B C8B 120.8(3) . . ?
C13B C8B C9B 116.7(3) . . ?
C13B C8B C7B 119.3(4) . . ?
C9B C8B C7B 124.0(3) . . ?
C10B C9B C8B 119.9(4) . . ?
C9B C10B C11B 118.9(4) . . ?
N12B C11B C10B 123.6(4) . . ?
C11B N12B C13B 117.2(3) . . ?
C11B N12B Cu1 130.7(3) . . ?
C13B N12B Cu1 111.8(2) . . ?
N12B C13B C8B 123.6(4) . . ?
N12B C13B C14B 116.4(3) . . ?
C8B C13B C14B 120.0(3) . . ?
N1B C14B C5B 123.3(4) . . ?
N1B C14B C13B 116.3(3) . . ?
C5B C14B C13B 120.4(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
Cu1 O11 1.968(3) . ?
Cu1 N1B 2.002(3) . ?
Cu1 N1A 2.005(4) . ?
Cu1 N12B 2.038(3) . ?
Cu1 N12A 2.251(3) . ?
C1 O13 1.266(6) . ?
C1 O12 1.280(5) . ?
C1 O11 1.308(4) . ?
N1A C2A 1.335(5) . ?
N1A C14A 1.374(5) . ?
C2A C3A 1.390(6) . ?
C3A C4A 1.374(6) . ?
C4A C5A 1.403(6) . ?
C5A C14A 1.391(6) . ?
C5A C6A 1.445(6) . ?
C6A C7A 1.323(7) . ?
C7A C8A 1.420(7) . ?
C8A C9A 1.407(6) . ?
C8A C13A 1.420(5) . ?
C9A C10A 1.362(7) . ?
C10A C11A 1.411(6) . ?
C11A N12A 1.329(5) . ?
N12A C13A 1.352(5) . ?
C13A C14A 1.453(5) . ?
N1B C2B 1.330(5) . ?
N1B C14B 1.369(4) . ?
C2B C3B 1.392(6) . ?
C3B C4B 1.378(6) . ?
C4B C5B 1.401(6) . ?
C5B C14B 1.394(5) . ?
C5B C6B 1.449(5) . ?
C6B C7B 1.360(6) . ?
C7B C8B 1.427(5) . ?
C8B C13B 1.400(5) . ?
C8B C9B 1.410(6) . ?
C9B C10B 1.361(6) . ?
C10B C11B 1.404(6) . ?
C11B N12B 1.316(5) . ?
N12B C13B 1.367(5) . ?
C13B C14B 1.435(5) . ?
