#------------------------------------------------------------------------------
#$Date: 2016-03-26 20:51:55 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180452 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/21/7212144.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_7212144
loop_
_publ_author_name
'Delgado, Fernando S.'
'Sanchiz, Joaquín'
'López, Trinidad'
'Lloret, Francesc'
'Julve, Miguel'
'Ruiz-Pérez, Catalina'
_publ_section_title
;
 Building-block process for the synthesis of new chromium(iii) malonate
 complexes
;
_journal_issue                   10
_journal_name_full               CrystEngComm
_journal_page_first              2711
_journal_paper_doi               10.1039/b920650g
_journal_volume                  12
_journal_year                    2010
_chemical_formula_sum            'C36 H98 Cl4 Cr2 Cu4 N16 O42'
_chemical_formula_weight         1927.26
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 102.637(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.7161(4)
_cell_length_b                   11.3208(10)
_cell_length_c                   20.1947(14)
_cell_measurement_temperature    293(2)
_cell_volume                     3729.1(4)
_computing_cell_refinement
'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.895
_diffrn_measured_fraction_theta_max 0.895
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           Mok\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0285
_diffrn_reflns_av_sigmaI/netI    0.0614
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            23087
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         6.40
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    1.649
_exptl_absorpt_correction_T_max  0.597
_exptl_absorpt_correction_T_min  0.412
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            'dark blue'
_exptl_crystal_density_diffrn    1.716
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1988
_exptl_crystal_size_max          0.68
_exptl_crystal_size_mid          0.48
_exptl_crystal_size_min          0.34
_refine_diff_density_max         1.225
_refine_diff_density_min         -1.401
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     470
_refine_ls_number_reflns         9739
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.1193
_refine_ls_R_factor_gt           0.0629
_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)+(0.1010P)²+7.4274P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1682
_refine_ls_wR_factor_ref         0.1997
_reflns_number_gt                5835
_reflns_number_total             9739
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b920650g.txt
_cod_data_source_block           compound3
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7212144
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
Cr1 Cr 0.06841(4) 0.05533(6) 0.05111(3) 0.01820(16) Uani 1 1 d .
C1 C -0.0040(3) 0.2909(4) 0.0391(2) 0.0234(9) Uani 1 1 d .
C2 C 0.0612(3) 0.3307(4) 0.0020(2) 0.0247(9) Uani 1 1 d .
H1 H 0.0435 0.3095 -0.0455 0.030 Uiso 1 1 calc R
H2 H 0.0652 0.4161 0.0046 0.030 Uiso 1 1 calc R
C3 C 0.1448(3) 0.2795(4) 0.0287(2) 0.0220(9) Uani 1 1 d .
O1 O -0.00068(18) 0.1902(3) 0.06603(15) 0.0246(6) Uani 1 1 d .
O2 O 0.15335(17) 0.1719(3) 0.04628(16) 0.0236(6) Uani 1 1 d .
O3 O -0.0603(2) 0.3622(3) 0.04013(19) 0.0351(8) Uani 1 1 d .
O4 O 0.20665(19) 0.3426(3) 0.03183(18) 0.0312(7) Uani 1 1 d .
C11 C 0.1815(3) -0.1420(4) 0.0833(3) 0.0317(10) Uani 1 1 d .
C12 C 0.1441(3) -0.1600(5) 0.1444(3) 0.0369(11) Uani 1 1 d .
H11 H 0.0908 -0.1966 0.1292 0.044 Uiso 1 1 calc R
H12 H 0.1783 -0.2151 0.1749 0.044 Uiso 1 1 calc R
C13 C 0.1336(3) -0.0518(4) 0.1836(2) 0.0309(10) Uani 1 1 d .
O11 O 0.15014(18) -0.0640(3) 0.04029(15) 0.0262(7) Uani 1 1 d .
O12 O 0.1060(2) 0.0428(3) 0.15022(15) 0.0292(7) Uani 1 1 d .
O13 O 0.2400(3) -0.2035(4) 0.0770(2) 0.0592(12) Uani 1 1 d .
O14 O 0.1498(3) -0.0542(4) 0.24593(18) 0.0527(11) Uani 1 1 d .
O20 O 0.01951(17) 0.0598(3) -0.04595(14) 0.0234(6) Uani 1 1 d .
H20 H 0.0553 0.0501 -0.0674 0.035 Uiso 1 1 calc R
Cu1 Cu -0.13999(3) 0.34609(5) 0.09877(3) 0.03053(16) Uani 1 1 d .
Cu2 Cu 0.30941(3) 0.25572(5) 0.07554(3) 0.02672(15) Uani 1 1 d .
N31 N -0.2382(3) 0.4206(5) 0.0289(3) 0.0520(13) Uani 1 1 d .
H30 H -0.2202 0.4774 0.0046 0.062 Uiso 1 1 calc R
H31 H -0.2641 0.3650 0.0001 0.062 Uiso 1 1 calc R
N32 N -0.1529(3) 0.1656(4) 0.1028(3) 0.0432(11) Uani 1 1 d .
H36 H -0.1631 0.1354 0.0606 0.052 Uiso 1 1 calc R
H37 H -0.1063 0.1332 0.1266 0.052 Uiso 1 1 calc R
N33 N -0.0663(3) 0.4483(6) 0.1710(3) 0.076(2) Uani 1 1 d .
H42 H -0.0137 0.4249 0.1768 0.092 Uiso 1 1 calc R
H43 H -0.0696 0.5245 0.1581 0.092 Uiso 1 1 calc R
N34 N -0.2194(3) 0.3480(4) 0.1633(2) 0.0420(11) Uani 1 1 d .
C31 C -0.2940(4) 0.4707(6) 0.0687(4) 0.065(2) Uani 1 1 d .
H33 H -0.3476 0.4846 0.0397 0.078 Uiso 1 1 calc R
H32 H -0.2726 0.5454 0.0887 0.078 Uiso 1 1 calc R
C32 C -0.3004(4) 0.3824(7) 0.1242(4) 0.0626(19) Uani 1 1 d .
H34 H -0.3317 0.4172 0.1545 0.075 Uiso 1 1 calc R
H35 H -0.3295 0.3127 0.1038 0.075 Uiso 1 1 calc R
C33 C -0.2207(4) 0.1378(5) 0.1352(4) 0.0568(17) Uani 1 1 d .
H39 H -0.2138 0.0590 0.1546 0.068 Uiso 1 1 calc R
H38 H -0.2723 0.1404 0.1020 0.068 Uiso 1 1 calc R
C34 C -0.2211(5) 0.2259(6) 0.1892(4) 0.068(2) Uani 1 1 d .
H41 H -0.1736 0.2134 0.2259 0.081 Uiso 1 1 calc R
H40 H -0.2698 0.2152 0.2072 0.081 Uiso 1 1 calc R
C35 C -0.0941(5) 0.4346(8) 0.2338(4) 0.075(2) Uani 1 1 d .
H45 H -0.0737 0.4993 0.2644 0.090 Uiso 1 1 calc R
H44 H -0.0733 0.3613 0.2559 0.090 Uiso 1 1 calc R
C36 C -0.1857(5) 0.4338(7) 0.2183(4) 0.072(2) Uani 1 1 d .
H46 H -0.2046 0.4130 0.2589 0.087 Uiso 1 1 calc R
H47 H -0.2060 0.5123 0.2044 0.087 Uiso 1 1 calc R
N51 N 0.3099(4) 0.1526(8) -0.0073(3) 0.092(3) Uani 1 1 d .
H50 H 0.2618 0.1141 -0.0194 0.111 Uiso 1 1 calc R
H51 H 0.3159 0.1983 -0.0423 0.111 Uiso 1 1 calc R
N52 N 0.2772(3) 0.2394(4) 0.1677(2) 0.0425(11) Uani 1 1 d .
H56 H 0.2948 0.3024 0.1940 0.051 Uiso 1 1 calc R
H57 H 0.2224 0.2343 0.1618 0.051 Uiso 1 1 calc R
N53 N 0.3975(3) 0.3937(5) 0.0852(3) 0.0613(15) Uani 1 1 d .
H62 H 0.4080 0.4113 0.0445 0.074 Uiso 1 1 calc R
H63 H 0.3787 0.4591 0.1022 0.074 Uiso 1 1 calc R
N54 N 0.4072(3) 0.1527(4) 0.1197(2) 0.0412(11) Uani 1 1 d .
C51 C 0.3763(6) 0.0684(7) 0.0082(4) 0.076(2) Uani 1 1 d .
H53 H 0.4218 0.0975 -0.0097 0.091 Uiso 1 1 calc R
H52 H 0.3583 -0.0055 -0.0145 0.091 Uiso 1 1 calc R
C52 C 0.4049(6) 0.0457(7) 0.0813(5) 0.089(3) Uani 1 1 d .
H54 H 0.3686 -0.0105 0.0960 0.107 Uiso 1 1 calc R
H55 H 0.4594 0.0113 0.0897 0.107 Uiso 1 1 calc R
C53 C 0.3157(4) 0.1331(6) 0.1987(3) 0.0556(16) Uani 1 1 d .
H58 H 0.3132 0.1308 0.2462 0.067 Uiso 1 1 calc R
H59 H 0.2871 0.0644 0.1764 0.067 Uiso 1 1 calc R
C54 C 0.3990(5) 0.1317(8) 0.1924(4) 0.077(2) Uani 1 1 d .
H61 H 0.4231 0.0559 0.2078 0.092 Uiso 1 1 calc R
H60 H 0.4292 0.1923 0.2215 0.092 Uiso 1 1 calc R
C55 C 0.4703(4) 0.3517(6) 0.1306(4) 0.065(2) Uani 1 1 d .
H65 H 0.4674 0.3704 0.1769 0.078 Uiso 1 1 calc R
H64 H 0.5175 0.3924 0.1208 0.078 Uiso 1 1 calc R
C56 C 0.4817(4) 0.2220(7) 0.1246(4) 0.067(2) Uani 1 1 d .
H66 H 0.5036 0.2069 0.0847 0.081 Uiso 1 1 calc R
H67 H 0.5221 0.1953 0.1639 0.081 Uiso 1 1 calc R
Cl1 Cl 0.61888(10) 0.29837(15) 0.32691(7) 0.0517(4) Uani 1 1 d .
O21 O 0.6802(13) 0.2218(15) 0.3528(10) 0.301(10) Uani 1 1 d .
O22 O 0.6254(6) 0.3273(16) 0.2654(4) 0.229(7) Uani 1 1 d .
O23 O 0.6390(5) 0.3792(8) 0.3797(5) 0.148(4) Uani 1 1 d .
O24 O 0.5450(5) 0.2395(9) 0.3281(4) 0.146(4) Uani 1 1 d .
Cl2 Cl 0.5003(3) -0.3018(2) 0.0863(2) 0.1459(16) Uani 1 1 d D
O25 O 0.5237(7) -0.3721(9) 0.0462(5) 0.177(5) Uani 1 1 d D
O26 O 0.4508(12) -0.2201(10) 0.0492(10) 0.87(6) Uani 1 1 d D
O27 O 0.4521(10) -0.3506(10) 0.1219(7) 0.276(10) Uani 1 1 d D
O28 O 0.5542(8) -0.2459(19) 0.1209(6) 0.348(16) Uani 1 1 d D
O1W O 0.3605(7) -0.1841(11) 0.2153(6) 0.183(4) Uani 1 1 d .
O2W O 0.4921(5) -0.3348(7) 0.2740(4) 0.125(3) Uani 1 1 d .
O3W O 0.3839(4) -0.0745(7) 0.3430(3) 0.107(2) Uani 1 1 d .
O4W O 0.2410(4) 0.0661(4) 0.3595(3) 0.0841(17) Uani 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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cr Cr 0.3209 0.6236 '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'
O O 0.0106 0.0060 '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'
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
O20 Cr1 O20 79.56(13) 3
O20 Cr1 O2 174.20(13) 3
O20 Cr1 O2 94.66(12) .
O20 Cr1 O11 93.94(13) 3
O20 Cr1 O11 93.14(13) .
O2 Cr1 O11 85.88(13) .
O20 Cr1 O12 94.31(13) 3
O20 Cr1 O12 173.52(13) .
O2 Cr1 O12 91.48(13) .
O11 Cr1 O12 89.34(13) .
O20 Cr1 O1 93.78(13) 3
O20 Cr1 O1 90.14(13) .
O2 Cr1 O1 86.63(12) .
O11 Cr1 O1 172.04(13) .
O12 Cr1 O1 88.16(13) .
O3 C1 O1 122.9(4) .
O3 C1 C2 116.3(4) .
O1 C1 C2 120.8(4) .
C3 C2 C1 114.9(4) .
O4 C3 O2 119.7(4) .
O4 C3 C2 119.6(4) .
O2 C3 C2 120.7(4) .
C1 O1 Cr1 127.3(3) .
C3 O2 Cr1 128.6(3) .
C1 O3 Cu1 124.2(3) .
C3 O4 Cu2 111.2(3) .
O13 C11 O11 122.9(5) .
O13 C11 C12 119.2(4) .
O11 C11 C12 118.0(4) .
C13 C12 C11 116.2(4) .
O14 C13 O12 121.7(5) .
O14 C13 C12 120.1(4) .
O12 C13 C12 118.2(4) .
C11 O11 Cr1 126.5(3) .
C13 O12 Cr1 126.0(3) .
O3 Cu1 N33 89.7(2) .
O3 Cu1 N34 173.67(17) .
N33 Cu1 N34 85.0(2) .
O3 Cu1 N32 101.90(16) .
N33 Cu1 N32 125.8(3) .
N34 Cu1 N32 84.08(17) .
O3 Cu1 N31 95.21(17) .
N33 Cu1 N31 120.9(3) .
N34 Cu1 N31 84.4(2) .
N32 Cu1 N31 110.6(2) .
O4 Cu2 N51 94.3(2) .
O4 Cu2 N54 174.38(15) .
N51 Cu2 N54 83.4(2) .
O4 Cu2 N52 94.24(16) .
N51 Cu2 N52 137.7(3) .
N54 Cu2 N52 84.07(19) .
O4 Cu2 N53 100.91(17) .
N51 Cu2 N53 111.7(3) .
N54 Cu2 N53 84.7(2) .
N52 Cu2 N53 107.2(2) .
C31 N31 Cu1 106.5(4) .
C33 N32 Cu1 109.3(3) .
C35 N33 Cu1 107.7(4) .
C32 N34 C34 110.6(6) .
C32 N34 C36 112.5(5) .
C34 N34 C36 112.3(6) .
C32 N34 Cu1 108.1(4) .
C34 N34 Cu1 106.2(3) .
C36 N34 Cu1 106.8(4) .
N31 C31 C32 107.7(5) .
N34 C32 C31 111.4(5) .
N32 C33 C34 108.3(5) .
C33 C34 N34 111.5(5) .
N33 C35 C36 109.1(6) .
N34 C36 C35 111.3(5) .
C51 N51 Cu2 109.9(4) .
C53 N52 Cu2 106.8(4) .
C55 N53 Cu2 106.8(4) .
C52 N54 C56 114.4(6) .
C52 N54 C54 113.1(6) .
C56 N54 C54 105.9(6) .
C52 N54 Cu2 108.8(4) .
C56 N54 Cu2 108.2(4) .
C54 N54 Cu2 106.1(4) .
N51 C51 C52 113.5(6) .
N54 C52 C51 111.0(7) .
C54 C53 N52 108.8(5) .
C53 C54 N54 112.3(6) .
N53 C55 C56 112.4(6) .
N54 C56 C55 114.5(5) .
O22 Cl1 O21 108.2(11) .
O22 Cl1 O23 120.4(9) .
O21 Cl1 O23 95.1(10) .
O22 Cl1 O24 112.9(6) .
O21 Cl1 O24 106.4(12) .
O23 Cl1 O24 111.4(4) .
O28 Cl2 O25 114.3(9) .
O28 Cl2 O27 112.2(8) .
O25 Cl2 O27 113.6(7) .
O28 Cl2 O26 104.7(9) .
O25 Cl2 O26 108.4(8) .
O27 Cl2 O26 102.5(9) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cr1 O20 1.950(3) 3
Cr1 O20 1.953(3) .
Cr1 O2 1.956(3) .
Cr1 O11 1.967(3) .
Cr1 O12 1.967(3) .
Cr1 O1 1.977(3) .
C1 O3 1.243(5) .
C1 O1 1.259(5) .
C1 C2 1.519(6) .
C2 C3 1.501(6) .
C3 O4 1.246(5) .
C3 O2 1.268(5) .
O3 Cu1 1.975(3) .
O4 Cu2 2.008(3) .
C11 O13 1.230(6) .
C11 O11 1.269(5) .
C11 C12 1.514(7) .
C12 C13 1.489(7) .
C13 O14 1.229(6) .
C13 O12 1.296(5) .
Cu1 N33 2.049(6) .
Cu1 N34 2.053(4) .
Cu1 N32 2.058(4) .
Cu1 N31 2.094(5) .
Cu2 N51 2.041(5) .
Cu2 N54 2.046(4) .
Cu2 N52 2.055(4) .
Cu2 N53 2.126(5) .
N31 C31 1.472(8) .
N32 C33 1.461(7) .
N33 C35 1.452(10) .
N34 C32 1.464(8) .
N34 C34 1.480(7) .
N34 C36 1.490(8) .
C31 C32 1.524(10) .
C33 C34 1.479(9) .
C35 C36 1.495(11) .
N51 C51 1.445(10) .
N52 C53 1.441(8) .
N53 C55 1.435(8) .
N54 C52 1.434(9) .
N54 C56 1.458(8) .
N54 C54 1.524(9) .
C51 C52 1.471(12) .
C53 C54 1.425(11) .
C55 C56 1.489(10) .
Cl1 O22 1.312(7) .
Cl1 O21 1.356(13) .
Cl1 O23 1.389(7) .
Cl1 O24 1.408(7) .
Cl2 O28 1.193(9) .
Cl2 O25 1.257(7) .
Cl2 O27 1.312(9) .
Cl2 O26 1.353(14) .
