#------------------------------------------------------------------------------
#$Date: 2016-03-26 19:51:55 +0100 (Sat 26 de Mar de 2016) $
#$Revision: 180452 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/21/7212145.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_7212145
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            'C24 H64 Cr2 N8 Ni O26'
_chemical_formula_weight         1043.54
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                106.313(4)
_cell_angle_beta                 103.821(4)
_cell_angle_gamma                95.435(5)
_cell_formula_units_Z            1
_cell_length_a                   9.1804(5)
_cell_length_b                   9.6532(5)
_cell_length_c                   13.0261(6)
_cell_measurement_temperature    293(2)
_cell_volume                     1059.48(10)
_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 0.968
_diffrn_measured_fraction_theta_max 0.968
_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  0.0384
_diffrn_reflns_av_sigmaI/netI    0.0892
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            12468
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         6.41
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    1.043
_exptl_absorpt_correction_T_max  0.801
_exptl_absorpt_correction_T_min  0.689
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            'dark violet'
_exptl_crystal_density_diffrn    1.636
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             548
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.880
_refine_diff_density_min         -0.788
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     373
_refine_ls_number_reflns         5987
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.1165
_refine_ls_R_factor_gt           0.0542
_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)+(0.0654P)²+0.2130P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1160
_refine_ls_wR_factor_ref         0.1368
_reflns_number_gt                3564
_reflns_number_total             5987
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b920650g.txt
_cod_data_source_block           compound4
_cod_original_cell_volume        1059.48(9)
_cod_database_code               7212145
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
Cr1 Cr -0.05174(6) -0.04499(5) 0.08883(4) 0.02298(15) Uani 1 1 d .
C1 C 0.0603(4) -0.3155(3) 0.1068(3) 0.0260(7) Uani 1 1 d .
C2 C -0.0691(4) -0.3516(5) 0.1519(4) 0.0354(8) Uani 1 1 d .
C3 C -0.2183(4) -0.3070(4) 0.1100(3) 0.0296(7) Uani 1 1 d .
O1 O 0.0757(3) -0.1989(2) 0.0809(2) 0.0317(5) Uani 1 1 d .
O2 O -0.2206(3) -0.1890(3) 0.0867(2) 0.0331(5) Uani 1 1 d .
O3 O 0.1549(3) -0.4001(3) 0.0980(2) 0.0409(6) Uani 1 1 d .
O4 O -0.3372(3) -0.3881(3) 0.1020(3) 0.0498(7) Uani 1 1 d .
C11 C -0.1863(4) 0.2066(4) 0.1778(3) 0.0326(8) Uani 1 1 d .
C12 C -0.0454(5) 0.2615(4) 0.2733(4) 0.0394(9) Uani 1 1 d .
C13 C 0.0359(4) 0.1527(4) 0.3166(3) 0.0310(7) Uani 1 1 d .
O11 O -0.1937(3) 0.0942(3) 0.09934(18) 0.0306(5) Uani 1 1 d .
O12 O 0.0254(3) 0.0235(3) 0.25360(18) 0.0314(5) Uani 1 1 d .
O13 O -0.2945(4) 0.2765(3) 0.1782(2) 0.0567(8) Uani 1 1 d .
O14 O 0.1126(3) 0.1937(3) 0.4145(2) 0.0502(7) Uani 1 1 d .
O20 O -0.1104(3) -0.0876(3) -0.0720(2) 0.0277(6) Uani 1 1 d .
Ni1 Ni -0.5000 -1.0000 0.5000 0.02315(16) Uani 1 2 d S
C31 C -0.2142(4) -0.9845(6) 0.4439(3) 0.0414(10) Uani 1 1 d .
C32 C -0.3109(4) -0.9368(5) 0.3542(3) 0.0355(8) Uani 1 1 d .
C34 C -0.5617(4) -0.8645(4) 0.3199(3) 0.0327(8) Uani 1 1 d .
C33 C -0.5253(5) -0.7344(4) 0.4233(3) 0.0401(9) Uani 1 1 d .
C35 C -0.5580(4) -1.1094(4) 0.1299(3) 0.0313(7) Uani 1 1 d .
C36 C -0.5391(4) -1.1202(4) 0.2468(3) 0.0299(7) Uani 1 1 d .
N31 N -0.2627(3) -0.9341(4) 0.5464(3) 0.0337(7) Uani 1 1 d .
N32 N -0.5407(5) -0.7806(4) 0.5198(3) 0.0364(7) Uani 1 1 d .
N33 N -0.5965(4) -1.2584(4) 0.0488(3) 0.0318(7) Uani 1 1 d .
N34 N -0.4761(3) -0.9818(3) 0.3390(2) 0.0258(6) Uani 1 1 d .
O1W O -0.4303(4) -0.4966(4) 0.2581(3) 0.0706(10) Uani 1 1 d .
O2W O 0.2470(4) -0.6014(3) 0.1969(3) 0.0664(9) Uani 1 1 d .
O3W O 0.1925(6) -0.3946(4) 0.3867(4) 0.1083(15) Uani 1 1 d .
O4W O 0.1481(14) 0.4472(12) 0.5649(8) 0.358(9) Uani 1 1 d .
H1 H -0.080(5) -0.443(5) 0.146(3) 0.051(13) Uiso 1 1 d .
H2 H -0.042(4) -0.314(4) 0.225(3) 0.031(10) Uiso 1 1 d .
H11 H -0.056(5) 0.333(5) 0.336(4) 0.053(12) Uiso 1 1 d .
H12 H 0.021(5) 0.308(5) 0.261(4) 0.053(14) Uiso 1 1 d .
H20 H -0.122(6) -0.148(5) -0.098(4) 0.043(17) Uiso 1 1 d .
H30 H -0.243(4) -0.841(4) 0.578(3) 0.022(9) Uiso 1 1 d .
H31 H -0.210(4) -0.966(4) 0.597(3) 0.033(10) Uiso 1 1 d .
H32 H -0.103(5) -0.950(4) 0.455(3) 0.040(10) Uiso 1 1 d .
H33 H -0.225(5) -1.089(5) 0.419(3) 0.047(12) Uiso 1 1 d .
H34 H -0.292(5) -0.827(5) 0.378(3) 0.044(11) Uiso 1 1 d .
H35 H -0.294(4) -0.963(4) 0.284(3) 0.036(10) Uiso 1 1 d .
H36 H -0.637(6) -0.782(5) 0.526(3) 0.053(13) Uiso 1 1 d .
H37 H -0.482(5) -0.723(5) 0.569(4) 0.043(13) Uiso 1 1 d .
H38 H -0.594(5) -0.665(5) 0.415(3) 0.050(12) Uiso 1 1 d .
H39 H -0.422(5) -0.683(4) 0.446(3) 0.033(10) Uiso 1 1 d .
H40 H -0.661(5) -0.903(4) 0.301(3) 0.033(10) Uiso 1 1 d .
H41 H -0.542(4) -0.835(4) 0.264(3) 0.035(10) Uiso 1 1 d .
H42 H -0.532(5) -1.298(4) 0.065(3) 0.029(11) Uiso 1 1 d .
H43 H -0.674(4) -1.307(3) 0.055(2) 0.016(8) Uiso 1 1 d .
H44 H -0.623(4) -1.256(4) -0.016(3) 0.027(9) Uiso 1 1 d .
H45 H -0.464(4) -1.056(4) 0.120(3) 0.034(9) Uiso 1 1 d .
H46 H -0.640(4) -1.058(4) 0.106(3) 0.031(9) Uiso 1 1 d .
H47 H -0.482(5) -1.182(4) 0.256(3) 0.045(12) Uiso 1 1 d .
H48 H -0.632(4) -1.159(4) 0.248(3) 0.030(9) Uiso 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'
Cr Cr 0.3209 0.6236 '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'
Ni Ni 0.3393 1.1124 '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'
H H 0.0000 0.0000 '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
O20 Cr1 O11 89.21(11) . .
O20 Cr1 O20 79.45(13) . 2
O11 Cr1 O20 95.43(11) . 2
O20 Cr1 O2 94.01(11) . .
O11 Cr1 O2 85.86(10) . .
O20 Cr1 O2 173.30(11) 2 .
O20 Cr1 O1 92.20(11) . .
O11 Cr1 O1 174.17(9) . .
O20 Cr1 O1 90.38(11) 2 .
O2 Cr1 O1 88.40(9) . .
O20 Cr1 O12 172.10(11) . .
O11 Cr1 O12 89.12(9) . .
O20 Cr1 O12 93.03(11) 2 .
O2 Cr1 O12 93.57(10) . .
O1 Cr1 O12 90.23(10) . .
O3 C1 O1 120.6(3) . .
O3 C1 C2 119.0(3) . .
O1 C1 C2 120.4(3) . .
C3 C2 C1 118.5(3) . .
O4 C3 O2 122.1(3) . .
O4 C3 C2 117.9(3) . .
O2 C3 C2 120.0(3) . .
C1 O1 Cr1 129.4(2) . .
C3 O2 Cr1 130.2(2) . .
O11 C11 O13 121.4(3) . .
O11 C11 C12 120.0(3) . .
O13 C11 C12 118.6(3) . .
C11 C12 C13 119.0(3) . .
O14 C13 O12 121.6(3) . .
O14 C13 C12 117.8(3) . .
O12 C13 C12 120.6(3) . .
C11 O11 Cr1 128.6(2) . .
C13 O12 Cr1 125.9(2) . .
Cr1 O20 Cr1 100.55(13) . 2
N31 Ni1 N31 180.0 . 2_436
N31 Ni1 N32 92.68(16) . .
N31 Ni1 N32 87.32(16) 2_436 .
N31 Ni1 N32 87.32(16) . 2_436
N31 Ni1 N32 92.68(16) 2_436 2_436
N32 Ni1 N32 180.00 . 2_436
N31 Ni1 N34 81.61(10) . .
N31 Ni1 N34 98.39(10) 2_436 .
N32 Ni1 N34 80.94(11) . .
N32 Ni1 N34 99.06(11) 2_436 .
N31 Ni1 N34 98.39(10) . 2_436
N31 Ni1 N34 81.61(10) 2_436 2_436
N32 Ni1 N34 99.06(11) . 2_436
N32 Ni1 N34 80.94(11) 2_436 2_436
N34 Ni1 N34 180.0 . 2_436
N31 C31 C32 109.3(3) . .
N34 C32 C31 111.7(3) . .
N34 C34 C33 111.4(3) . .
N32 C33 C34 110.7(3) . .
N33 C35 C36 109.3(3) . .
N34 C36 C35 115.7(3) . .
C31 N31 Ni1 106.5(2) . .
C33 N32 Ni1 111.3(2) . .
C36 N34 C34 110.6(3) . .
C36 N34 C32 111.2(3) . .
C34 N34 C32 110.8(3) . .
C36 N34 Ni1 112.31(19) . .
C34 N34 Ni1 104.79(19) . .
C32 N34 Ni1 106.87(19) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cr1 O20 1.945(3) .
Cr1 O11 1.959(2) .
Cr1 O20 1.963(3) 2
Cr1 O2 1.971(2) .
Cr1 O1 1.972(2) .
Cr1 O12 1.983(2) .
C1 O3 1.250(4) .
C1 O1 1.268(4) .
C1 C2 1.499(5) .
C2 C3 1.499(5) .
C3 O4 1.246(4) .
C3 O2 1.259(4) .
C11 O11 1.247(4) .
C11 O13 1.253(4) .
C11 C12 1.494(5) .
C12 C13 1.502(5) .
C13 O14 1.230(4) .
C13 O12 1.266(4) .
O20 Cr1 1.963(3) 2
Ni1 N31 2.100(3) .
Ni1 N31 2.100(3) 2_436
Ni1 N32 2.140(3) .
Ni1 N32 2.140(3) 2_436
Ni1 N34 2.213(2) .
Ni1 N34 2.213(2) 2_436
C31 N31 1.475(5) .
C31 C32 1.500(5) .
C32 N34 1.487(4) .
C34 N34 1.482(4) .
C34 C33 1.503(5) .
C33 N32 1.479(5) .
C35 N33 1.477(5) .
C35 C36 1.524(5) .
C36 N34 1.478(4) .
