#------------------------------------------------------------------------------
#$Date: 2016-03-24 02:38:42 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179590 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/55/4505531.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_4505531
loop_
_publ_author_name
'Kirillov, Alexander M.'
'Karabach, Yauhen Y.'
'Kirillova, Marina V.'
'Haukka, Matti'
'Pombeiro, Armando J. L.'
_publ_section_title
;
 Topologically Unique 2D Heterometallic CuII/Mg Coordination Polymer:
 Synthesis, Structural Features, and Catalytic Use in Alkane
 Hydrocarboxylation
;
_journal_issue                   3
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              1069
_journal_paper_doi               10.1021/cg201459k
_journal_volume                  12
_journal_year                    2012
_chemical_formula_moiety         'C11 H20 Cu Mg N O10, H4 O2, H2 O'
_chemical_formula_sum            'C11 H26 Cu Mg N O13'
_chemical_formula_weight         468.18
_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                96.271(2)
_cell_angle_beta                 114.843(2)
_cell_angle_gamma                115.2440(10)
_cell_formula_units_Z            2
_cell_length_a                   10.4720(3)
_cell_length_b                   10.5610(3)
_cell_length_c                   11.0590(4)
_cell_measurement_reflns_used    11765
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.00
_cell_volume                     939.88(6)
_computing_cell_refinement       'Denzo/Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'Denzo/Scalepack (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'Diamond v.3.1b (Crystal Impact GbR, 2006)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'φ scans and ω scans with κ offset'
_diffrn_radiation_monochromator  'horizontally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0363
_diffrn_reflns_av_sigmaI/netI    0.0410
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            18184
_diffrn_reflns_theta_full        27.56
_diffrn_reflns_theta_max         27.56
_diffrn_reflns_theta_min         3.52
_exptl_absorpt_coefficient_mu    1.262
_exptl_absorpt_correction_T_max  0.9396
_exptl_absorpt_correction_T_min  0.7837
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Xprep in Shelxtl v.6.14-1 (Sheldrick, 2005)'
_exptl_crystal_colour            'pale blue'
_exptl_crystal_density_diffrn    1.654
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             488
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.348
_refine_diff_density_min         -0.502
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     265
_refine_ls_number_reflns         4287
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0509
_refine_ls_R_factor_gt           0.0408
_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)+(0.0503P)²+1.8655P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1003
_refine_ls_wR_factor_ref         0.1062
_reflns_number_gt                3672
_reflns_number_total             4287
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg201459k_si_001.cif
_cod_data_source_block           compound-1
_cod_original_cell_volume        939.88(5)
_cod_database_code               4505531
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
Cu1 Cu 0.78533(4) 0.10567(3) 0.61259(3) 0.01209(11) Uani 1 1 d .
Mg1 Mg 1.0000 0.0000 0.5000 0.0068(2) Uani 1 2 d S
Mg2 Mg 1.0000 0.0000 1.0000 0.0148(3) Uani 1 2 d S
O1 O 0.9934(2) 0.15283(19) 0.6234(2) 0.0133(4) Uani 1 1 d .
O2 O 0.6135(2) 0.0603(2) 0.3809(2) 0.0164(4) Uani 1 1 d .
H2O H 0.5026 -0.0031 0.3358 0.025 Uiso 1 1 d R
O3 O 0.6888(2) 0.1273(2) 0.7248(2) 0.0159(4) Uani 1 1 d .
O4 O 0.6927(2) -0.1034(2) 0.5909(2) 0.0151(4) Uani 1 1 d .
O5 O 0.8606(2) -0.1600(2) 0.5539(2) 0.0160(4) Uani 1 1 d .
O6 O 0.7824(3) -0.0406(3) 0.3198(2) 0.0274(5) Uani 1 1 d .
H6C H 0.7247 -0.1180 0.2345 0.041 Uiso 1 1 d R
H6D H 0.7213 -0.0037 0.3351 0.041 Uiso 1 1 d R
O7 O 0.8496(2) -0.2019(2) 0.8345(2) 0.0170(4) Uani 1 1 d .
O8 O 0.6589(3) -0.3455(2) 0.8814(2) 0.0266(5) Uani 1 1 d .
O9 O 1.1962(3) -0.0321(3) 1.0674(2) 0.0254(5) Uani 1 1 d .
H9A H 1.2162 -0.0741 1.1295 0.038 Uiso 1 1 d R
H9B H 1.2398 -0.0428 1.0188 0.038 Uiso 1 1 d R
O10 O 0.9168(3) -0.1079(2) 1.1194(2) 0.0269(5) Uani 1 1 d .
H10A H 0.9537 -0.0967 1.2112 0.040 Uiso 1 1 d R
H10B H 0.8221 -0.1880 1.0602 0.040 Uiso 1 1 d R
O11 O 0.9337(4) 0.2423(4) 0.2407(4) 0.0521(8) Uani 1 1 d .
H11A H 0.8577 0.1583 0.1853 0.078 Uiso 1 1 d R
H11B H 1.0047 0.2501 0.2248 0.078 Uiso 1 1 d R
N1 N 0.8507(3) 0.3166(2) 0.6244(2) 0.0150(5) Uani 1 1 d .
C1 C 1.1005(3) 0.3108(3) 0.6800(3) 0.0175(6) Uani 1 1 d .
H1A H 1.1870 0.3387 0.6553 0.021 Uiso 1 1 calc R
H1B H 1.1554 0.3460 0.7850 0.021 Uiso 1 1 calc R
C2 C 1.0045(4) 0.3855(3) 0.6210(4) 0.0265(7) Uani 1 1 d .
H2A H 1.0730 0.4935 0.6784 0.032 Uiso 1 1 calc R
H2B H 0.9773 0.3747 0.5219 0.032 Uiso 1 1 calc R
C3 C 0.6418(4) 0.2010(3) 0.3651(3) 0.0208(6) Uani 1 1 d .
H3A H 0.5366 0.1884 0.2932 0.025 Uiso 1 1 calc R
H3B H 0.7200 0.2364 0.3311 0.025 Uiso 1 1 calc R
C4 C 0.7118(4) 0.3156(4) 0.5053(4) 0.0268(7) Uani 1 1 d .
H4A H 0.7517 0.4160 0.4973 0.032 Uiso 1 1 calc R
H4B H 0.6233 0.2933 0.5267 0.032 Uiso 1 1 calc R
C5 C 0.7324(4) 0.2773(3) 0.7775(3) 0.0218(6) Uani 1 1 d .
H5A H 0.7643 0.3045 0.8786 0.026 Uiso 1 1 calc R
H5B H 0.6359 0.2867 0.7232 0.026 Uiso 1 1 calc R
C6 C 0.8749(4) 0.3834(3) 0.7641(4) 0.0291(7) Uani 1 1 d .
H6A H 0.8807 0.4801 0.7710 0.035 Uiso 1 1 calc R
H6B H 0.9802 0.4021 0.8426 0.035 Uiso 1 1 calc R
C7 C 0.7387(3) -0.1913(3) 0.5672(3) 0.0115(5) Uani 1 1 d .
C8 C 0.6233(3) -0.3520(3) 0.5395(3) 0.0112(5) Uani 1 1 d .
C9 C 0.5247(3) -0.4470(3) 0.3981(3) 0.0118(5) Uani 1 1 d .
H9 H 0.5424 -0.4108 0.3282 0.014 Uiso 1 1 calc R
C10 C 0.5993(3) -0.4058(3) 0.6429(3) 0.0120(5) Uani 1 1 d .
C11 C 0.7094(3) -0.3105(3) 0.7984(3) 0.0148(5) Uani 1 1 d .
O99 O 0.5442(7) -0.2445(8) 1.0525(6) 0.0528(17) Uani 0.50 1 d P
H99A H 0.5425 -0.2833 0.9839 0.079 Uiso 0.50 1 d PR
H99B H 0.4564 -0.2294 1.0183 0.079 Uiso 0.50 1 d PR
O98 O 0.3724(7) -0.0951(8) 0.9608(6) 0.0504(15) Uani 0.50 1 d P
H98A H 0.4287 0.0075 0.9792 0.076 Uiso 0.50 1 d PR
H98B H 0.2802 -0.1380 0.8597 0.076 Uiso 0.50 1 d PR
O97 O 0.3940(8) -0.1806(8) 0.9919(7) 0.0522(15) Uani 0.50 1 d P
H97A H 0.2785 -0.2381 0.8979 0.078 Uiso 0.50 1 d PR
H97B H 0.4725 -0.1373 0.9680 0.078 Uiso 0.50 1 d PR
O96 O 0.4981(8) -0.3846(7) 1.0464(8) 0.0586(18) Uani 0.50 1 d P
H96A H 0.5584 -0.3605 0.9957 0.088 Uiso 0.50 1 d PR
H96B H 0.4510 -0.4744 1.0192 0.088 Uiso 0.50 1 d PR
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'
Mg Mg 0.0486 0.0363 '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
O4 Cu1 O3 89.56(8) . . ?
O4 Cu1 O1 100.22(7) . . ?
O3 Cu1 O1 143.93(8) . . ?
O4 Cu1 N1 172.40(8) . . yes
O3 Cu1 N1 86.08(8) . . yes
O1 Cu1 N1 86.93(8) . . yes
O4 Cu1 O2 94.33(8) . . ?
O3 Cu1 O2 110.11(8) . . ?
O1 Cu1 O2 103.71(7) . . ?
N1 Cu1 O2 81.36(8) . . yes
O1 Mg1 O1 180.00(10) 2_756 . ?
O1 Mg1 O5 91.95(7) 2_756 . ?
O1 Mg1 O5 88.05(7) . . yes
O1 Mg1 O5 88.05(7) 2_756 2_756 ?
O1 Mg1 O5 91.95(7) . 2_756 ?
O5 Mg1 O5 180.00(9) . 2_756 ?
O1 Mg1 O6 89.53(8) 2_756 . ?
O1 Mg1 O6 90.46(8) . . yes
O5 Mg1 O6 90.48(8) . . ?
O5 Mg1 O6 89.51(8) 2_756 . ?
O1 Mg1 O6 90.47(8) 2_756 2_756 ?
O1 Mg1 O6 89.54(8) . 2_756 ?
O5 Mg1 O6 89.52(8) . 2_756 ?
O5 Mg1 O6 90.48(8) 2_756 2_756 ?
O6 Mg1 O6 180.00(14) . 2_756 ?
O7 Mg2 O7 180.0 2_757 . ?
O7 Mg2 O10 91.49(8) 2_757 . ?
O7 Mg2 O10 88.51(8) . . yes
O7 Mg2 O10 88.51(8) 2_757 2_757 ?
O7 Mg2 O10 91.49(8) . 2_757 ?
O10 Mg2 O10 180.000(1) . 2_757 ?
O7 Mg2 O9 89.22(8) 2_757 . ?
O7 Mg2 O9 90.78(8) . . ?
O10 Mg2 O9 93.66(9) . . yes
O10 Mg2 O9 86.34(9) 2_757 . ?
O7 Mg2 O9 90.78(8) 2_757 2_757 ?
O7 Mg2 O9 89.22(8) . 2_757 ?
O10 Mg2 O9 86.34(9) . 2_757 ?
O10 Mg2 O9 93.66(9) 2_757 2_757 ?
O9 Mg2 O9 180.00(6) . 2_757 ?
C1 O1 Cu1 108.26(15) . . ?
C1 O1 Mg1 127.48(16) . . ?
Cu1 O1 Mg1 120.11(9) . . ?
C3 O2 Cu1 107.86(16) . . ?
C3 O2 H2O 107.3 . . ?
Cu1 O2 H2O 122.2 . . ?
C5 O3 Cu1 112.11(16) . . ?
C7 O4 Cu1 130.00(17) . . ?
C7 O5 Mg1 135.92(17) . . ?
Mg1 O6 H6C 123.1 . . ?
Mg1 O6 H6D 118.0 . . ?
H6C O6 H6D 115.2 . . ?
C11 O7 Mg2 129.75(18) . . ?
Mg2 O9 H9A 121.1 . . ?
Mg2 O9 H9B 126.1 . . ?
H9A O9 H9B 108.0 . . ?
Mg2 O10 H10A 137.9 . . ?
Mg2 O10 H10B 107.0 . . ?
H10A O10 H10B 115.0 . . ?
H11A O11 H11B 101.1 . . ?
C2 N1 C4 113.3(2) . . ?
C2 N1 C6 113.0(2) . . ?
C4 N1 C6 110.7(2) . . ?
C2 N1 Cu1 107.62(17) . . ?
C4 N1 Cu1 109.02(18) . . ?
C6 N1 Cu1 102.64(17) . . ?
O1 C1 C2 110.5(2) . . ?
O1 C1 H1A 109.5 . . ?
C2 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 108.1 . . ?
N1 C2 C1 110.2(2) . . ?
N1 C2 H2A 109.6 . . ?
C1 C2 H2A 109.6 . . ?
N1 C2 H2B 109.6 . . ?
C1 C2 H2B 109.6 . . ?
H2A C2 H2B 108.1 . . ?
O2 C3 C4 110.6(2) . . ?
O2 C3 H3A 109.5 . . ?
C4 C3 H3A 109.5 . . ?
O2 C3 H3B 109.5 . . ?
C4 C3 H3B 109.5 . . ?
H3A C3 H3B 108.1 . . ?
N1 C4 C3 111.8(2) . . ?
N1 C4 H4A 109.3 . . ?
C3 C4 H4A 109.3 . . ?
N1 C4 H4B 109.3 . . ?
C3 C4 H4B 109.3 . . ?
H4A C4 H4B 107.9 . . ?
O3 C5 C6 110.7(2) . . ?
O3 C5 H5A 109.5 . . ?
C6 C5 H5A 109.5 . . ?
O3 C5 H5B 109.5 . . ?
C6 C5 H5B 109.5 . . ?
H5A C5 H5B 108.1 . . ?
N1 C6 C5 109.6(3) . . ?
N1 C6 H6A 109.7 . . ?
C5 C6 H6A 109.7 . . ?
N1 C6 H6B 109.7 . . ?
C5 C6 H6B 109.7 . . ?
H6A C6 H6B 108.2 . . ?
O5 C7 O4 126.8(2) . . yes
O5 C7 C8 118.2(2) . . ?
O4 C7 C8 114.7(2) . . ?
C9 C8 C10 119.5(2) . . ?
C9 C8 C7 116.0(2) . . ?
C10 C8 C7 124.2(2) . . ?
C8 C9 C10 121.3(2) . 2_646 ?
C8 C9 H9 119.4 . . ?
C10 C9 H9 119.4 2_646 . ?
C9 C10 C8 119.2(2) 2_646 . ?
C9 C10 C11 119.1(2) 2_646 . ?
C8 C10 C11 121.6(2) . . ?
O8 C11 O7 125.5(3) . . yes
O8 C11 C10 118.8(2) . . ?
O7 C11 C10 115.7(2) . . ?
H99A O99 H99B 107.1 . . ?
H99A O99 H96A 37.5 . . ?
H99B O99 H96A 130.2 . . ?
H98A O98 H98B 104.0 . . ?
H98A O98 H97A 163.4 . . ?
H98B O98 H97A 60.4 . . ?
H98A O98 H97B 106.1 . . ?
H98B O98 H97B 108.5 . . ?
H97A O98 H97B 76.2 . . ?
H99B O97 H97A 118.5 . . ?
H99B O97 H97B 75.7 . . ?
H97A O97 H97B 107.6 . . ?
H99A O96 H96A 42.1 . . ?
H99A O96 H96B 132.9 . . ?
H96A O96 H96B 101.7 . . ?
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 O4 1.9327(18) . yes
Cu1 O3 1.9498(19) . yes
Cu1 O1 1.9633(18) . yes
Cu1 N1 2.003(2) . yes
Cu1 O2 2.270(2) . yes
Mg1 O1 2.0404(18) 2_756 yes
Mg1 O1 2.0405(18) . yes
Mg1 O5 2.0465(18) . yes
Mg1 O5 2.0465(18) 2_756 yes
Mg1 O6 2.123(2) . yes
Mg1 O6 2.124(2) 2_756 yes
Mg2 O7 2.0587(19) 2_757 yes
Mg2 O7 2.0587(19) . yes
Mg2 O10 2.061(2) . yes
Mg2 O10 2.061(2) 2_757 yes
Mg2 O9 2.062(2) . yes
Mg2 O9 2.062(2) 2_757 yes
O1 C1 1.421(3) . ?
O2 C3 1.432(3) . ?
O2 H2O 0.9068 . ?
O3 C5 1.420(3) . ?
O4 C7 1.263(3) . yes
O5 C7 1.253(3) . yes
O6 H6C 0.9247 . ?
O6 H6D 0.9379 . ?
O7 C11 1.266(3) . yes
O8 C11 1.254(3) . yes
O9 H9A 0.8577 . ?
O9 H9B 0.8645 . ?
O10 H10A 0.8945 . ?
O10 H10B 0.8639 . ?
O11 H11A 0.8160 . ?
O11 H11B 0.8072 . ?
N1 C2 1.477(4) . ?
N1 C4 1.491(4) . ?
N1 C6 1.493(4) . ?
C1 C2 1.515(4) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.512(5) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.516(4) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.504(3) . ?
C8 C9 1.391(4) . ?
C8 C10 1.399(4) . ?
C9 C10 1.392(4) 2_646 ?
C9 H9 0.9500 . ?
C10 C9 1.392(4) 2_646 ?
C10 C11 1.505(4) . ?
O99 H99A 0.8115 . ?
O99 H99B 0.9264 . ?
O99 H96A 1.4089 . ?
O98 H98A 0.9327 . ?
O98 H98B 0.9983 . ?
O98 H97A 1.2887 . ?
O98 H97B 1.2807 . ?
O97 H99B 0.9695 . ?
O97 H97A 1.0442 . ?
O97 H97B 0.9181 . ?
O96 H99A 1.3579 . ?
O96 H96A 0.9842 . ?
O96 H96B 0.8048 . ?
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
_geom_hbond_publ_flag
O6 H6C O99 0.92 1.86 2.726(6) 154.3 1_554 yes
O6 H6C O96 0.92 2.60 3.466(8) 156.3 1_554 yes
O6 H6D O2 0.94 1.75 2.679(3) 173.6 . yes
O9 H9A O3 0.86 1.80 2.637(3) 165.5 2_757 yes
O9 H9B O98 0.86 1.99 2.818(6) 159.3 1_655 yes
O9 H9B O11 0.86 2.65 3.204(4) 123.3 2_756 yes
O10 H10A O1 0.89 1.92 2.763(3) 157.3 2_757 yes
O10 H10B O8 0.86 1.90 2.706(3) 154.4 . yes
O11 H11A O98 0.82 2.00 2.578(7) 127.8 2_656 yes
O2 H2O O3 0.91 1.62 2.520(3) 170.8 2_656 yes
