#------------------------------------------------------------------------------
#$Date: 2015-04-02 14:22:18 +0300 (Thu, 02 Apr 2015) $
#$Revision: 134621 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/01/4300172.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_4300172
loop_
_publ_author_name
'Rodolphe Clérac'
'F. Albert Cotton'
'Lee M. Daniels'
'Kim R. Dunbar'
'Carlos A. Murillo'
'Isabel Pascual'
_publ_section_title
;
Linear Trichromium Complexes with Direct Cr to Cr Contacts. 2. Compounds
with Cr3(dipyridylamide)43+ Cores
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              752
_journal_page_last               756
_journal_paper_doi               10.1021/ic991022t
_journal_volume                  39
_journal_year                    2000
_chemical_compound_source        synthesis
_chemical_formula_structural     Cr3(N3C10H8)4Cl2.Cl.2(CH2Cl2).OC4H8
_chemical_formula_sum            'C46 H44 Cl7 Cr3 N12 O'
_chemical_formula_weight         1185.08
_space_group_IT_number           73
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-I 2b 2c'
_symmetry_space_group_name_H-M   'I b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.122(1)
_cell_length_b                   17.151(1)
_cell_length_c                   37.508(2)
_cell_measurement_reflns_used    186
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      20.8
_cell_measurement_theta_min      8.2
_cell_volume                     10371.3(10)
_computing_cell_refinement       MADNES
_computing_data_collection       MADNES
_computing_data_reduction        PROCOR
_computing_molecular_graphics    'XP - Siemens, 1996'
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measurement_device       'Nonius FAST'
_diffrn_measurement_method       'Ellipsoid mask fitting'
_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  0.0575
_diffrn_reflns_av_sigmaI/netI    0.0272
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            21811
_diffrn_reflns_theta_max         22.57
_diffrn_reflns_theta_min         2.37
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    1.027
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.518
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             4824
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.540
_refine_diff_density_min         -0.429
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.069
_refine_ls_goodness_of_fit_obs   1.064
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     333
_refine_ls_number_reflns         3397
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_restrained_S_obs      1.064
_refine_ls_R_factor_all          0.0752
_refine_ls_R_factor_obs          0.0640
_refine_ls_shift/esd_max         0.004
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1000P)²+80.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1848
_refine_ls_wR_factor_obs         0.1656
_reflns_number_observed          2859
_reflns_number_total             3403
_reflns_observed_criterion       >2sigma(I)
_cod_depositor_comments
;
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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+80.0000P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+80.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        10371(1)
_cod_database_code               4300172
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-x+1/2, y+1, -z+1'
'x+1, -y+1, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'x+1/2, -y, z'
'-x, 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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Cr1 Cr 0.38796(5) 0.16738(5) 0.34940(2) 0.0267(3) Uani 1 d . .
Cr2 Cr 0.4890(7) 0.2465(13) 0.35010(4) 0.025(2) Uani 0.50 d P -1
Cl1 Cl 0.27270(9) 0.08322(8) 0.34828(4) 0.0403(4) Uani 1 d . .
N1 N 0.3210(2) 0.2632(2) 0.36982(11) 0.0288(10) Uani 1 d . .
N2 N 0.4468(3) 0.3151(3) 0.38728(11) 0.0293(10) Uani 1 d . .
N3 N 0.5758(3) 0.3622(2) 0.40114(11) 0.0313(10) Uani 1 d . .
N4 N 0.3694(3) 0.2055(3) 0.29686(11) 0.0302(10) Uani 1 d . .
N5 N 0.4457(3) 0.3133(2) 0.31266(10) 0.0278(10) Uani 1 d . .
N6 N 0.5295(3) 0.4164(2) 0.32891(11) 0.0317(10) Uani 1 d . .
C1 C 0.2376(3) 0.2696(3) 0.36553(15) 0.0365(13) Uani 1 d . .
H1 H 0.2092(3) 0.2286(3) 0.35426(15) 0.044 Uiso 1 calc R .
C2 C 0.1929(4) 0.3327(3) 0.3768(2) 0.0435(15) Uani 1 d . .
H2 H 0.1351(4) 0.3346(3) 0.3735(2) 0.052 Uiso 1 calc R .
C3 C 0.2348(4) 0.3937(4) 0.3930(2) 0.050(2) Uani 1 d . .
H3 H 0.2056(4) 0.4380(4) 0.4009(2) 0.060 Uiso 1 calc R .
C4 C 0.3191(4) 0.3891(3) 0.3977(2) 0.0424(15) Uani 1 d . .
H4 H 0.3478(4) 0.4306(3) 0.4084(2) 0.051 Uiso 1 calc R .
C5 C 0.3619(3) 0.3233(3) 0.38646(14) 0.0307(12) Uani 1 d . .
C6 C 0.4962(3) 0.3501(3) 0.41213(15) 0.0324(12) Uani 1 d . .
C7 C 0.4728(4) 0.3670(4) 0.4469(2) 0.045(2) Uani 1 d . .
H7 H 0.4176(4) 0.3591(4) 0.4541(2) 0.053 Uiso 1 calc R .
C8 C 0.5299(4) 0.3953(4) 0.4709(2) 0.057(2) Uani 1 d . .
H8 H 0.5143(4) 0.4065(4) 0.4945(2) 0.068 Uiso 1 calc R .
C9 C 0.6108(4) 0.4071(4) 0.4598(2) 0.049(2) Uani 1 d . .
H9 H 0.6508(4) 0.4271(4) 0.4755(2) 0.059 Uiso 1 calc R .
C10 C 0.6314(4) 0.3893(4) 0.42558(15) 0.0406(14) Uani 1 d . .
H10 H 0.6868(4) 0.3960(4) 0.41841(15) 0.049 Uiso 1 calc R .
C11 C 0.3350(3) 0.1596(4) 0.2716(2) 0.0403(14) Uani 1 d . .
H11 H 0.3116(3) 0.1119(4) 0.2787(2) 0.048 Uiso 1 calc R .
C12 C 0.3324(4) 0.1790(4) 0.23578(15) 0.0423(15) Uani 1 d . .
H12 H 0.3074(4) 0.1459(4) 0.21897(15) 0.051 Uiso 1 calc R .
C13 C 0.3678(4) 0.2486(4) 0.22569(15) 0.046(2) Uani 1 d . .
H13 H 0.3680(4) 0.2632(4) 0.20153(15) 0.055 Uiso 1 calc R .
C14 C 0.4026(3) 0.2965(4) 0.25051(15) 0.0398(14) Uani 1 d . .
H14 H 0.4262(3) 0.3442(4) 0.24352(15) 0.048 Uiso 1 calc R .
C15 C 0.4032(3) 0.2744(3) 0.28648(14) 0.0300(12) Uani 1 d . .
C16 C 0.4587(3) 0.3923(3) 0.31231(13) 0.0300(12) Uani 1 d . .
C17 C 0.4007(4) 0.4472(3) 0.3000(2) 0.0380(14) Uani 1 d . .
H17 H 0.3516(4) 0.4303(3) 0.2889(2) 0.046 Uiso 1 calc R .
C18 C 0.4158(4) 0.5251(3) 0.3041(2) 0.045(2) Uani 1 d . .
H18 H 0.3775(4) 0.5620(3) 0.2956(2) 0.054 Uiso 1 calc R .
C19 C 0.4875(4) 0.5491(3) 0.3208(2) 0.046(2) Uani 1 d . .
H19 H 0.4985(4) 0.6025(3) 0.3241(2) 0.055 Uiso 1 calc R .
C20 C 0.5418(4) 0.4948(3) 0.3325(2) 0.0409(14) Uani 1 d . .
H20 H 0.5907(4) 0.5118(3) 0.3437(2) 0.049 Uiso 1 calc R .
Cl2 Cl 0.5000 0.2500 0.14994(5) 0.0425(5) Uani 1 d S .
C21 C 0.5797(6) 0.1178(6) 0.0919(2) 0.089(3) Uani 1 d . .
Cl2A Cl 0.4811(9) 0.0872(17) 0.0763(5) 0.177(10) Uani 0.37(3) d P 1
Cl3A Cl 0.6510(3) 0.0981(10) 0.05783(13) 0.090(3) Uani 0.63(3) d P 1
Cl2B Cl 0.4925(5) 0.0679(4) 0.0777(2) 0.083(2) Uani 0.63(3) d P 2
Cl3B Cl 0.6443(10) 0.1498(18) 0.0576(3) 0.109(5) Uani 0.37(3) d P 2
O1 O 0.3140(12) 0.3874(11) 0.5098(5) 0.123(5) Uiso 0.50 d P -1
C22 C 0.3325(16) 0.3080(14) 0.5192(6) 0.099(7) Uiso 0.50 d P -1
C23 C 0.2428(16) 0.2650(13) 0.5124(5) 0.103(7) Uiso 0.50 d P -1
C24 C 0.2130(18) 0.3187(16) 0.4858(7) 0.110(7) Uiso 0.50 d P -1
C25 C 0.2410(30) 0.4060(9) 0.4977(13) 0.095(7) Uiso 0.50 d P -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'
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'
O O 0.0106 0.0060 '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
Cr1 Cr2 Cr1 176.6(9) . 6_554 ?
N3 Cr1 N4 171.2(2) 6_554 . ?
N3 Cr1 N6 89.8(2) 6_554 6_554 ?
N4 Cr1 N6 87.7(2) . 6_554 ?
N3 Cr1 N1 89.7(2) 6_554 . ?
N4 Cr1 N1 91.4(2) . . ?
N6 Cr1 N1 171.1(2) 6_554 . ?
N3 Cr1 Cr2 85.9(2) 6_554 . ?
N4 Cr1 Cr2 85.5(2) . . ?
N6 Cr1 Cr2 87.4(5) 6_554 . ?
N1 Cr1 Cr2 83.7(5) . . ?
N3 Cr1 Cl1 95.09(12) 6_554 . ?
N4 Cr1 Cl1 93.53(12) . . ?
N6 Cr1 Cl1 94.26(12) 6_554 . ?
N1 Cr1 Cl1 94.60(12) . . ?
Cr2 Cr1 Cl1 178.0(5) . . ?
N5 Cr2 N2 92.0(9) . . ?
N5 Cr2 N2 170.3(7) . 6_554 ?
N2 Cr2 N2 90.0(3) . 6_554 ?
N5 Cr2 N5 89.1(2) . 6_554 ?
N2 Cr2 N5 168.6(7) . 6_554 ?
N2 Cr2 N5 87.0(8) 6_554 6_554 ?
N5 Cr2 Cr1 95.3(4) . . ?
N2 Cr2 Cr1 97.3(4) . . ?
N2 Cr2 Cr1 93.9(7) 6_554 . ?
N5 Cr2 Cr1 93.8(7) 6_554 . ?
N5 Cr2 Cr1 85.9(6) . 6_554 ?
N2 Cr2 Cr1 85.8(6) . 6_554 ?
N2 Cr2 Cr1 84.8(4) 6_554 6_554 ?
N5 Cr2 Cr1 83.0(4) 6_554 6_554 ?
C1 N1 C5 117.9(5) . . ?
C1 N1 Cr1 121.8(4) . . ?
C5 N1 Cr1 120.3(3) . . ?
C6 N2 C5 123.4(4) . . ?
C6 N2 Cr2 123.5(5) . . ?
C5 N2 Cr2 113.1(4) . . ?
C6 N3 C10 117.9(4) . . ?
C6 N3 Cr1 120.5(3) . 6_554 ?
C10 N3 Cr1 121.5(4) . 6_554 ?
C11 N4 C15 118.1(5) . . ?
C11 N4 Cr1 122.4(4) . . ?
C15 N4 Cr1 118.9(3) . . ?
C16 N5 C15 123.5(4) . . ?
C16 N5 Cr2 122.4(6) . . ?
C15 N5 Cr2 114.2(6) . . ?
C16 N6 C20 117.6(5) . . ?
C16 N6 Cr1 119.3(3) . 6_554 ?
C20 N6 Cr1 123.0(4) . 6_554 ?
N1 C1 C2 123.4(5) . . ?
C1 C2 C3 118.5(5) . . ?
C4 C3 C2 119.6(6) . . ?
C3 C4 C5 120.1(6) . . ?
N1 C5 N2 114.3(4) . . ?
N1 C5 C4 120.6(5) . . ?
N2 C5 C4 124.8(5) . . ?
N3 C6 N2 114.1(4) . . ?
N3 C6 C7 120.5(5) . . ?
N2 C6 C7 125.1(5) . . ?
C8 C7 C6 120.5(5) . . ?
C7 C8 C9 118.9(6) . . ?
C10 C9 C8 118.8(6) . . ?
C9 C10 N3 123.4(5) . . ?
N4 C11 C12 123.6(6) . . ?
C13 C12 C11 117.6(5) . . ?
C14 C13 C12 120.4(5) . . ?
C13 C14 C15 119.9(6) . . ?
N4 C15 N5 114.8(4) . . ?
N4 C15 C14 120.5(5) . . ?
N5 C15 C14 124.1(5) . . ?
N6 C16 N5 115.0(4) . . ?
N6 C16 C17 120.3(5) . . ?
N5 C16 C17 124.3(5) . . ?
C18 C17 C16 120.0(6) . . ?
C17 C18 C19 119.5(5) . . ?
C20 C19 C18 119.0(6) . . ?
C19 C20 N6 123.6(6) . . ?
Cl2B C21 Cl3B 114.4(7) . . ?
Cl3A C21 Cl2A 106.9(7) . . ?
C25 O1 C22 120.4(22) . . ?
O1 C22 C23 101.8(19) . . ?
C24 C23 C22 96.5(21) . . ?
C23 C24 C25 107.8(25) . . ?
O1 C25 C24 97.0(22) . . ?
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
Cr1 Cr2 2.120(14) . ?
Cr2 Cr1 2.474(13) 6_554 ?
Cr1 N3 2.089(4) 6_554 ?
Cr1 N4 2.098(4) . ?
Cr1 N6 2.103(4) 6_554 ?
Cr1 N1 2.110(4) . ?
Cr1 Cl1 2.353(2) . ?
Cr2 N5 1.943(15) . ?
Cr2 N2 1.95(2) . ?
Cr2 N5 2.033(15) 6_554 ?
N1 C1 1.360(7) . ?
N1 C5 1.373(7) . ?
N2 C6 1.364(7) . ?
N2 C5 1.377(7) . ?
N3 C6 1.363(7) . ?
N3 C10 1.364(7) . ?
N4 C11 1.351(7) . ?
N4 C15 1.359(7) . ?
N5 C16 1.371(7) . ?
N5 C15 1.371(7) . ?
N6 C16 1.364(7) . ?
N6 C20 1.366(7) . ?
C1 C2 1.365(8) . ?
C2 C3 1.388(9) . ?
C3 C4 1.371(9) . ?
C4 C5 1.389(8) . ?
C6 C7 1.387(8) . ?
C7 C8 1.377(9) . ?
C8 C9 1.384(9) . ?
C9 C10 1.359(8) . ?
C11 C12 1.384(8) . ?
C12 C13 1.376(9) . ?
C13 C14 1.362(9) . ?
C14 C15 1.402(8) . ?
C16 C17 1.404(8) . ?
C17 C18 1.366(9) . ?
C18 C19 1.379(9) . ?
C19 C20 1.352(9) . ?
C21 Cl2B 1.730(12) . ?
C21 Cl3B 1.745(14) . ?
C21 Cl3A 1.752(10) . ?
C21 Cl2A 1.77(2) . ?
O1 C25 1.30(6) . ?
O1 C22 1.44(3) . ?
C22 C23 1.64(3) . ?
C23 C24 1.44(3) . ?
C24 C25 1.63(4) . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 Cr1 Cr1 N3 47.3(2) . . 6_554 . ?
N4 Cr1 Cr1 N6 49.0(2) . . 6_554 . ?
