#------------------------------------------------------------------------------
#$Date: 2016-03-25 15:58:18 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179945 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/40/7024073.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_7024073
loop_
_publ_author_name
'Dean, Rebecca K.'
'Granville, Stephanie L.'
'Dawe, Louise N.'
'Decken, Andreas'
'Hattenhauer, Karen M.'
'Kozak, Christopher M.'
_publ_section_title
;
 Structure and magnetic behaviour of mono- and bimetallic chromium(III)
 complexes of amine-bis(phenolate) ligands.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              548
_journal_page_last               559
_journal_paper_doi               10.1039/b910254j
_journal_volume                  39
_journal_year                    2010
_chemical_formula_moiety         'C48 H54 Cl2 Cr2 N4 O5, C7 H8'
_chemical_formula_sum            'C55 H62 Cl2 Cr2 N4 O5'
_chemical_formula_weight         1033.99
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      13
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/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                 108.533(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.222(3)
_cell_length_b                   13.867(3)
_cell_length_c                   14.612(3)
_cell_measurement_reflns_used    5572
_cell_measurement_temperature    198(1)
_cell_measurement_theta_max      28.24
_cell_measurement_theta_min      2.28
_cell_volume                     2732.3(10)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'Bruker SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      198(1)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'Bruker AXS SMART1000/P4'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0573
_diffrn_reflns_av_sigmaI/netI    0.0798
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18165
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.47
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              K760
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.544
_exptl_absorpt_correction_T_max  0.9733
_exptl_absorpt_correction_T_min  0.8119
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2004)'
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.257
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1084
_exptl_crystal_recrystallization_method 'CHLOROFORM, TOLUENE'
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.097
_refine_diff_density_min         -0.580
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         6028
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.1339
_refine_ls_R_factor_gt           0.0701
_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)+(0.1469P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2174
_refine_ls_wR_factor_ref         0.2609
_reflns_number_gt                3105
_reflns_number_total             6028
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            b910254j.txt
_cod_data_source_block           cmpd_5
_cod_original_cell_volume        2732.2(9)
_cod_original_sg_symbol_H-M      'P 2/n'
_cod_database_code               7024073
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, 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 0.33955(6) 0.52448(6) 0.17950(5) 0.0414(3) Uani 1 1 d .
Cl1 Cl 0.21637(10) 0.53941(10) 0.02826(8) 0.0532(4) Uani 1 1 d .
O1 O 0.3645(2) 0.3939(2) 0.1540(2) 0.0435(8) Uani 1 1 d .
O2 O 0.3155(3) 0.6597(2) 0.2152(2) 0.0508(9) Uani 1 1 d .
O3 O 0.2500 0.4799(3) 0.2500 0.0416(11) Uani 1 2 d S
N1 N 0.4658(3) 0.5134(3) 0.3018(3) 0.0418(10) Uani 1 1 d .
N2 N 0.4476(3) 0.5728(3) 0.1223(3) 0.0467(11) Uani 1 1 d .
C1 C 0.3928(4) 0.7250(4) 0.2441(3) 0.0505(13) Uani 1 1 d .
C2 C 0.3839(5) 0.8146(4) 0.2003(4) 0.0621(16) Uani 1 1 d .
C3 C 0.4669(5) 0.8751(4) 0.2284(4) 0.0683(17) Uani 1 1 d .
H3 H 0.4628 0.9369 0.1994 0.082 Uiso 1 1 calc R
C4 C 0.5546(5) 0.8479(5) 0.2971(4) 0.0686(18) Uani 1 1 d .
C5 C 0.5606(5) 0.7584(4) 0.3390(4) 0.0616(16) Uani 1 1 d .
H5 H 0.6205 0.7391 0.3864 0.074 Uiso 1 1 calc R
C6 C 0.4800(4) 0.6958(4) 0.3130(3) 0.0528(14) Uani 1 1 d .
C7 C 0.2882(5) 0.8441(5) 0.1259(5) 0.077(2) Uani 1 1 d .
H7A H 0.2647 0.7918 0.0791 0.115 Uiso 1 1 calc R
H7B H 0.2992 0.9022 0.0925 0.115 Uiso 1 1 calc R
H7C H 0.2384 0.8575 0.1577 0.115 Uiso 1 1 calc R
C8 C 0.6424(6) 0.9161(6) 0.3233(6) 0.096(2) Uani 1 1 d .
H8A H 0.6540 0.9406 0.3889 0.144 Uiso 1 1 calc R
H8B H 0.6286 0.9701 0.2778 0.144 Uiso 1 1 calc R
H8C H 0.7015 0.8815 0.3203 0.144 Uiso 1 1 calc R
C9 C 0.3841(3) 0.3213(4) 0.2174(3) 0.0401(11) Uani 1 1 d .
C10 C 0.3523(4) 0.2286(4) 0.1832(4) 0.0488(13) Uani 1 1 d .
C11 C 0.3741(5) 0.1524(4) 0.2463(4) 0.0605(15) Uani 1 1 d .
H11 H 0.3522 0.0899 0.2223 0.073 Uiso 1 1 calc R
C12 C 0.4269(5) 0.1627(4) 0.3442(4) 0.0600(16) Uani 1 1 d .
C13 C 0.4547(4) 0.2537(4) 0.3767(3) 0.0493(13) Uani 1 1 d .
H13 H 0.4902 0.2627 0.4432 0.059 Uiso 1 1 calc R
C14 C 0.4335(4) 0.3340(4) 0.3166(3) 0.0414(12) Uani 1 1 d .
C15 C 0.2927(5) 0.2146(4) 0.0792(4) 0.0613(16) Uani 1 1 d .
H15A H 0.3363 0.2192 0.0393 0.092 Uiso 1 1 calc R
H15B H 0.2415 0.2646 0.0596 0.092 Uiso 1 1 calc R
H15C H 0.2612 0.1509 0.0706 0.092 Uiso 1 1 calc R
C16 C 0.4499(6) 0.0772(5) 0.4110(5) 0.093(3) Uani 1 1 d .
H16A H 0.5189 0.0576 0.4230 0.140 Uiso 1 1 calc R
H16B H 0.4057 0.0237 0.3814 0.140 Uiso 1 1 calc R
H16C H 0.4400 0.0947 0.4723 0.140 Uiso 1 1 calc R
C17 C 0.4585(4) 0.4297(4) 0.3652(3) 0.0448(12) Uani 1 1 d .
H17A H 0.5227 0.4236 0.4175 0.054 Uiso 1 1 calc R
H17B H 0.4075 0.4454 0.3959 0.054 Uiso 1 1 calc R
C18 C 0.4821(4) 0.6016(4) 0.3640(3) 0.0500(13) Uani 1 1 d .
H18A H 0.5471 0.5955 0.4151 0.060 Uiso 1 1 calc R
H18B H 0.4305 0.6034 0.3963 0.060 Uiso 1 1 calc R
C19 C 0.5518(4) 0.4949(4) 0.2663(3) 0.0514(14) Uani 1 1 d .
H19A H 0.5566 0.4248 0.2555 0.062 Uiso 1 1 calc R
H19B H 0.6138 0.5152 0.3163 0.062 Uiso 1 1 calc R
C20 C 0.5422(4) 0.5476(4) 0.1745(3) 0.0499(14) Uani 1 1 d .
C21 C 0.6215(4) 0.5626(5) 0.1421(4) 0.0610(16) Uani 1 1 d .
H21 H 0.6861 0.5426 0.1798 0.073 Uiso 1 1 calc R
C22 C 0.6058(5) 0.6079(5) 0.0525(4) 0.0628(17) Uani 1 1 d .
H22 H 0.6591 0.6181 0.0275 0.075 Uiso 1 1 calc R
C23 C 0.5108(5) 0.6372(4) 0.0018(4) 0.0618(16) Uani 1 1 d .
H23 H 0.4986 0.6701 -0.0579 0.074 Uiso 1 1 calc R
C24 C 0.4333(4) 0.6191(4) 0.0374(3) 0.0540(14) Uani 1 1 d .
H24 H 0.3683 0.6397 0.0013 0.065 Uiso 1 1 calc R
C25 C 0.3421(7) 0.8364(8) 0.8420(7) 0.064(3) Uani 0.50 1 d PD
C26 C 0.2536(8) 0.8077(8) 0.8550(8) 0.076(4) Uani 0.50 1 d PD
C27 C 0.1966(5) 0.7344(6) 0.7993(5) 0.086(2) Uani 1 1 d D
C28 C 0.2177(7) 0.7029(11) 0.7177(7) 0.094(5) Uani 0.50 1 d PD
C29 C 0.3664(8) 0.7986(8) 0.7644(7) 0.069(3) Uani 0.50 1 d PD
C30 C 0.4096(12) 0.9103(10) 0.9094(9) 0.089(5) Uani 0.50 1 d P
H30A H 0.3754 0.9725 0.9024 0.134 Uiso 0.50 1 calc PR
H30B H 0.4707 0.9176 0.8926 0.134 Uiso 0.50 1 calc PR
H30C H 0.4260 0.8880 0.9763 0.134 Uiso 0.50 1 calc 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'
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'
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
O1 Cr1 O3 89.77(16) . .
O1 Cr1 O2 176.38(13) . .
O3 Cr1 O2 88.00(17) . .
O1 Cr1 N2 91.14(16) . .
O3 Cr1 N2 172.72(11) . .
O2 Cr1 N2 90.71(16) . .
O1 Cr1 N1 86.27(15) . .
O3 Cr1 N1 93.00(11) . .
O2 Cr1 N1 91.00(15) . .
N2 Cr1 N1 79.85(15) . .
O1 Cr1 Cl1 91.67(10) . .
O3 Cr1 Cl1 96.11(5) . .
O2 Cr1 Cl1 91.40(10) . .
N2 Cr1 Cl1 91.08(12) . .
N1 Cr1 Cl1 170.65(12) . .
C9 O1 Cr1 126.2(3) . .
C1 O2 Cr1 120.5(3) . .
Cr1 O3 Cr1 143.5(3) 2 .
C19 N1 C18 111.5(4) . .
C19 N1 C17 107.7(4) . .
C18 N1 C17 106.4(4) . .
C19 N1 Cr1 106.9(3) . .
C18 N1 Cr1 112.5(3) . .
C17 N1 Cr1 111.8(3) . .
C24 N2 C20 117.9(4) . .
C24 N2 Cr1 127.3(4) . .
C20 N2 Cr1 114.6(3) . .
O2 C1 C2 120.0(5) . .
O2 C1 C6 118.1(5) . .
C2 C1 C6 121.7(5) . .
C1 C2 C3 117.3(6) . .
C1 C2 C7 120.4(6) . .
C3 C2 C7 122.3(6) . .
C4 C3 C2 122.1(6) . .
C4 C3 H3 118.9 . .
C2 C3 H3 118.9 . .
C5 C4 C3 118.9(6) . .
C5 C4 C8 121.4(7) . .
C3 C4 C8 119.7(6) . .
C4 C5 C6 120.9(6) . .
C4 C5 H5 119.6 . .
C6 C5 H5 119.6 . .
C1 C6 C5 119.1(5) . .
C1 C6 C18 119.1(5) . .
C5 C6 C18 121.6(5) . .
C2 C7 H7A 109.5 . .
C2 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
C2 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
C4 C8 H8A 109.5 . .
C4 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
C4 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
O1 C9 C10 118.1(4) . .
O1 C9 C14 123.1(4) . .
C10 C9 C14 118.7(4) . .
C11 C10 C9 119.3(5) . .
C11 C10 C15 121.1(5) . .
C9 C10 C15 119.6(5) . .
C10 C11 C12 122.9(6) . .
C10 C11 H11 118.5 . .
C12 C11 H11 118.5 . .
C13 C12 C11 117.0(5) . .
C13 C12 C16 121.6(6) . .
C11 C12 C16 121.3(6) . .
C12 C13 C14 122.7(5) . .
C12 C13 H13 118.6 . .
C14 C13 H13 118.6 . .
C13 C14 C9 119.2(5) . .
C13 C14 C17 116.1(4) . .
C9 C14 C17 124.5(4) . .
C10 C15 H15A 109.5 . .
C10 C15 H15B 109.5 . .
H15A C15 H15B 109.5 . .
C10 C15 H15C 109.5 . .
H15A C15 H15C 109.5 . .
H15B C15 H15C 109.5 . .
C12 C16 H16A 109.5 . .
C12 C16 H16B 109.5 . .
H16A C16 H16B 109.5 . .
C12 C16 H16C 109.5 . .
H16A C16 H16C 109.5 . .
H16B C16 H16C 109.5 . .
C14 C17 N1 116.3(4) . .
C14 C17 H17A 108.2 . .
N1 C17 H17A 108.2 . .
C14 C17 H17B 108.2 . .
N1 C17 H17B 108.2 . .
H17A C17 H17B 107.4 . .
N1 C18 C6 115.7(4) . .
N1 C18 H18A 108.4 . .
C6 C18 H18A 108.4 . .
N1 C18 H18B 108.4 . .
C6 C18 H18B 108.4 . .
H18A C18 H18B 107.4 . .
N1 C19 C20 112.1(4) . .
N1 C19 H19A 109.2 . .
C20 C19 H19A 109.2 . .
N1 C19 H19B 109.2 . .
C20 C19 H19B 109.2 . .
H19A C19 H19B 107.9 . .
N2 C20 C21 122.8(5) . .
N2 C20 C19 114.8(4) . .
C21 C20 C19 122.2(5) . .
C20 C21 C22 119.1(6) . .
C20 C21 H21 120.5 . .
C22 C21 H21 120.5 . .
C23 C22 C21 118.0(5) . .
C23 C22 H22 121.0 . .
C21 C22 H22 121.0 . .
C22 C23 C24 120.5(5) . .
C22 C23 H23 119.8 . .
C24 C23 H23 119.8 . .
N2 C24 C23 121.6(5) . .
N2 C24 H24 119.2 . .
C23 C24 H24 119.2 . .
C29 C25 C26 118.3(10) . .
C29 C25 C30 120.7(9) . .
C26 C25 C30 121.0(9) . .
C25 C26 C27 121.0(9) . .
C25 C26 C29 116.9(8) . 2_556
C28 C27 C26 119.2(9) . .
C29 C27 C28 119.8(9) 2_556 2_556
C27 C28 C27 119.7(9) . 2_556
C27 C28 C29 116.1(10) 2_556 2_556
C27 C29 C25 120.9(10) 2_556 .
C25 C30 H30A 109.5 . .
C25 C30 H30B 109.5 . .
H30A C30 H30B 109.5 . .
C25 C30 H30C 109.5 . .
H30A C30 H30C 109.5 . .
H30B C30 H30C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cr1 O1 1.905(3) .
Cr1 O3 1.9745(16) .
Cr1 O2 2.004(4) .
Cr1 N2 2.080(4) .
Cr1 N1 2.098(4) .
Cr1 Cl1 2.3526(14) .
O1 C9 1.337(5) .
O2 C1 1.383(6) .
O3 Cr1 1.9745(16) 2
N1 C19 1.494(6) .
N1 C18 1.498(6) .
N1 C17 1.510(6) .
N2 C24 1.354(6) .
N2 C20 1.364(7) .
C1 C2 1.384(8) .
C1 C6 1.387(7) .
C2 C3 1.399(8) .
C2 C7 1.504(8) .
C3 C4 1.381(9) .
C3 H3 0.9500 .
C4 C5 1.375(8) .
C4 C8 1.514(9) .
C5 C6 1.391(7) .
C5 H5 0.9500 .
C6 C18 1.500(7) .
C7 H7A 0.9800 .
C7 H7B 0.9800 .
C7 H7C 0.9800 .
C8 H8A 0.9800 .
C8 H8B 0.9800 .
C8 H8C 0.9800 .
C9 C10 1.402(7) .
C9 C14 1.407(6) .
C10 C11 1.370(7) .
C10 C15 1.500(7) .
C11 C12 1.396(8) .
C11 H11 0.9500 .
C12 C13 1.362(8) .
C12 C16 1.504(8) .
C13 C14 1.390(7) .
C13 H13 0.9500 .
C14 C17 1.494(7) .
C15 H15A 0.9800 .
C15 H15B 0.9800 .
C15 H15C 0.9800 .
C16 H16A 0.9800 .
C16 H16B 0.9800 .
C16 H16C 0.9800 .
C17 H17A 0.9900 .
C17 H17B 0.9900 .
C18 H18A 0.9900 .
C18 H18B 0.9900 .
C19 C20 1.495(6) .
C19 H19A 0.9900 .
C19 H19B 0.9900 .
C20 C21 1.369(8) .
C21 C22 1.406(7) .
C21 H21 0.9500 .
C22 C23 1.380(8) .
C22 H22 0.9500 .
C23 C24 1.383(8) .
C23 H23 0.9500 .
C24 H24 0.9500 .
C25 C29 1.3900(10) .
C25 C26 1.3900(11) .
C25 C30 1.529(15) .
C26 C27 1.3901(10) .
C27 C29 1.3896(10) 2_556
C27 C28 1.3900(11) .
C27 C28 1.3902(11) 2_556
C28 C27 1.3902(11) 2_556
C29 C27 1.3896(10) 2_556
C30 H30A 0.9800 .
C30 H30B 0.9800 .
C30 H30C 0.9800 .
