#------------------------------------------------------------------------------
#$Date: 2021-10-29 14:47:48 +0300 (Fri, 29 Oct 2021) $
#$Revision: 270159 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/11/70/4117038.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_4117038
loop_
_publ_author_name
'Cotton, F. Albert'
'Daniels, Lee M.'
'Murillo, Carlos A.'
'Pascual, Isabel'
_publ_section_title
;
 Compounds with Linear, Bonded Trichromium Chains
;
_journal_coden_ASTM              JACSAT
_journal_issue                   42
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10223
_journal_page_last               10224
_journal_paper_doi               10.1021/ja971998+
_journal_volume                  119
_journal_year                    1997
_chemical_formula_sum            'C41 H34 B Cl3 Cr3 F4 N12'
_chemical_formula_weight         1043.97
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 110.920(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.114(2)
_cell_length_b                   16.7460(10)
_cell_length_c                   15.6554(10)
_cell_measurement_reflns_used    192
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      17.7
_cell_measurement_theta_min      9.0
_cell_volume                     4680.7(7)
_computing_cell_refinement       MADNES
_computing_data_collection       MADNES
_computing_data_reduction        PROCOR
_computing_molecular_graphics    XPW
_computing_publication_material  'CIFTAB, 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       'Frame data from ω scans'
_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  0.0510
_diffrn_reflns_av_sigmaI/netI    0.0313
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10557
_diffrn_reflns_theta_max         22.46
_diffrn_reflns_theta_min         2.43
_diffrn_standards_number         'none (Area detector)'
_exptl_absorpt_coefficient_mu    1.033
_exptl_absorpt_correction_type   'none (N/A)'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.602
_exptl_crystal_description       'regular block'
_exptl_crystal_F_000             2280
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.474
_refine_diff_density_min         -0.339
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.053
_refine_ls_goodness_of_fit_obs   1.065
_refine_ls_hydrogen_treatment    free
_refine_ls_matrix_type           full
_refine_ls_number_parameters     401
_refine_ls_number_reflns         2984
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_restrained_S_obs      1.065
_refine_ls_R_factor_all          0.0378
_refine_ls_R_factor_obs          0.0353
_refine_ls_shift/esd_max         0.004
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0431P)²+12.9920P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0907
_refine_ls_wR_factor_obs         0.0881
_reflns_number_observed          2782
_reflns_number_total             2984
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja9719982B_2.cif
_cod_data_source_block           cmpd2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0431P)^2^+12.9920P] 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^)+(0.0431P)^2^+12.9920P] 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        4680.7(6)
_cod_database_code               4117038
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Cr1 Cr 0.5000 0.62929(4) 0.2500 0.0195(2) Uani 1 d S .
Cr2 Cr 0.5000 0.78710(4) 0.2500 0.0183(2) Uani 1 d S .
Cr3 Cr 0.5000 0.90625(4) 0.2500 0.0211(2) Uani 1 d S .
Cl1 Cl 0.5000 0.47821(6) 0.2500 0.0363(3) Uani 1 d S .
B1 B 0.5000 1.1303(4) 0.2500 0.052(2) Uani 1 d S .
F1 F 0.5000 1.0480(2) 0.2500 0.0435(7) Uani 1 d S .
F2 F 0.5765(4) 1.1509(4) 0.3078(12) 0.108(2) Uani 0.50 d P -1
F3 F 0.4583(9) 1.1617(6) 0.2882(13) 0.121(7) Uani 0.50 d P -1
F4 F 0.4932(16) 1.1539(6) 0.1680(10) 0.160(7) Uani 0.50 d P -1
N1 N 0.54894(13) 0.64503(13) 0.3964(2) 0.0211(5) Uani 1 d . .
N2 N 0.57352(13) 0.77921(13) 0.3805(2) 0.0210(5) Uani 1 d . .
N3 N 0.60362(13) 0.90747(13) 0.3552(2) 0.0212(5) Uani 1 d . .
N4 N 0.60917(13) 0.64291(13) 0.2439(2) 0.0212(5) Uani 1 d . .
N5 N 0.58563(13) 0.77657(13) 0.2028(2) 0.0209(5) Uani 1 d . .
N6 N 0.55873(13) 0.90811(13) 0.1606(2) 0.0219(5) Uani 1 d . .
C1 C 0.5512(2) 0.5813(2) 0.4509(2) 0.0268(7) Uani 1 d . .
C2 C 0.5752(2) 0.5853(2) 0.5446(2) 0.0348(8) Uani 1 d . .
C3 C 0.5938(2) 0.6592(2) 0.5859(2) 0.0363(8) Uani 1 d . .
C4 C 0.5922(2) 0.7249(2) 0.5331(2) 0.0293(7) Uani 1 d . .
C5 C 0.57326(15) 0.7166(2) 0.4379(2) 0.0206(6) Uani 1 d . .
C6 C 0.6540(2) 0.9677(2) 0.3668(2) 0.0258(7) Uani 1 d . .
C7 C 0.7243(2) 0.9656(2) 0.4312(2) 0.0318(8) Uani 1 d . .
C8 C 0.7444(2) 0.8998(2) 0.4890(2) 0.0312(7) Uani 1 d . .
C9 C 0.6949(2) 0.8385(2) 0.4790(2) 0.0280(7) Uani 1 d . .
C10 C 0.62413(15) 0.8410(2) 0.4084(2) 0.0202(6) Uani 1 d . .
C11 C 0.6564(2) 0.5793(2) 0.2650(2) 0.0298(7) Uani 1 d . .
C12 C 0.7297(2) 0.5827(2) 0.2717(2) 0.0377(8) Uani 1 d . .
C13 C 0.7587(2) 0.6562(2) 0.2605(2) 0.0366(8) Uani 1 d . .
C14 C 0.7127(2) 0.7218(2) 0.2398(2) 0.0294(7) Uani 1 d . .
C15 C 0.6362(2) 0.7140(2) 0.2271(2) 0.0212(6) Uani 1 d . .
C16 C 0.5637(2) 0.9737(2) 0.1120(2) 0.0262(7) Uani 1 d . .
C17 C 0.6026(2) 0.9746(2) 0.0545(2) 0.0343(8) Uani 1 d . .
C18 C 0.6365(2) 0.9049(2) 0.0415(2) 0.0350(8) Uani 1 d . .
C19 C 0.6329(2) 0.8374(2) 0.0900(2) 0.0305(7) Uani 1 d . .
C20 C 0.5949(2) 0.8399(2) 0.1517(2) 0.0212(6) Uani 1 d . .
C21 C 0.5981(2) 0.6757(3) -0.0967(3) 0.0489(9) Uani 1 d . .
Cl2 Cl 0.62052(6) 0.63072(5) 0.01116(7) 0.0565(3) Uani 1 d . .
Cl3A Cl 0.6738(2) 0.6564(6) -0.1366(2) 0.089(2) Uani 0.595(15) d P .
Cl3 Cl 0.6759(3) 0.7158(11) -0.1133(7) 0.123(4) Uani 0.405(15) d P .
H4 H 0.6009(17) 0.7748(19) 0.5573(20) 0.022(8) Uiso 1 d . .
H8 H 0.7906(20) 0.8998(18) 0.5321(23) 0.031(9) Uiso 1 d . .
H11 H 0.6366(16) 0.5346(18) 0.2757(19) 0.021(8) Uiso 1 d . .
H9 H 0.7090(16) 0.7945(17) 0.5178(20) 0.018(7) Uiso 1 d . .
H18 H 0.6629(18) 0.9020(18) 0.0017(21) 0.029(8) Uiso 1 d . .
H6 H 0.6357(18) 1.0081(21) 0.3264(23) 0.035(9) Uiso 1 d . .
H1 H 0.5372(18) 0.5360(20) 0.4199(21) 0.030(9) Uiso 1 d . .
H17 H 0.6033(18) 1.0174(21) 0.0251(22) 0.034(9) Uiso 1 d . .
H13 H 0.8099(20) 0.6623(19) 0.2658(22) 0.037(9) Uiso 1 d . .
H16 H 0.5394(16) 1.0176(19) 0.1203(19) 0.022(8) Uiso 1 d . .
H3 H 0.6038(19) 0.6652(19) 0.6465(26) 0.037(9) Uiso 1 d . .
H2 H 0.5752(18) 0.5403(20) 0.5770(23) 0.035(9) Uiso 1 d . .
H14 H 0.7299(18) 0.7698(19) 0.2325(20) 0.026(8) Uiso 1 d . .
H19 H 0.6510(18) 0.7911(20) 0.0782(22) 0.030(9) Uiso 1 d . .
H8 H 0.7543(19) 1.0053(21) 0.4348(22) 0.036(9) Uiso 1 d . .
H21A H 0.5660(31) 0.6437(30) -0.1341(38) 0.091(18) Uiso 1 d . .
H12 H 0.7601(23) 0.5367(23) 0.2862(27) 0.059(11) Uiso 1 d . .
H22A H 0.5794(23) 0.7293(27) -0.1030(27) 0.058(12) Uiso 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'
B B 0.0013 0.0007 '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'
F F 0.0171 0.0103 '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
N4 Cr1 N4 167.74(12) 2_655 .
N4 Cr1 N1 89.95(8) . 2_655
N4 Cr1 N1 88.56(8) . .
N1 Cr1 N1 165.99(12) 2_655 .
N4 Cr1 Cl1 96.13(6) . .
N1 Cr1 Cl1 97.00(6) . .
N4 Cr1 Cr2 83.87(6) . .
N1 Cr1 Cr2 83.00(6) . .
Cl1 Cr1 Cr2 180.0 . .
Cr3 Cr2 N5 94.99(6) . 2_655
Cr3 Cr2 N2 93.73(6) . 2_655
N5 Cr2 N2 90.14(9) 2_655 2_655
Cr3 Cr2 N5 94.99(6) . .
N5 Cr2 N5 170.03(13) 2_655 .
N2 Cr2 N5 89.22(9) 2_655 .
Cr3 Cr2 N2 93.73(6) . .
N2 Cr2 N2 172.54(13) 2_655 .
N5 Cr2 N2 90.13(9) . .
Cr3 Cr2 Cr1 180.0 . .
N5 Cr2 Cr1 85.01(6) . .
N2 Cr2 Cr1 86.27(6) . .
Cr2 Cr3 N3 90.56(6) . .
N3 Cr3 N3 178.87(12) . 2_655
Cr2 Cr3 N6 90.86(6) . .
N3 Cr3 N6 86.71(9) . .
N3 Cr3 N6 93.27(9) 2_655 .
N6 Cr3 N6 178.28(12) 2_655 .
Cr2 Cr3 F1 180.0 . .
N3 Cr3 F1 89.44(6) . .
N6 Cr3 F1 89.14(6) . .
F3 B1 F3 131.0(11) . 2_655
F3 B1 F4 118.6(6) . .
F3 B1 F4 118.6(6) 2_655 2_655
F4 B1 F4 144.8(12) . 2_655
F3 B1 F1 114.5(6) . .
F3 B1 F1 114.5(6) 2_655 .
F4 B1 F1 107.6(6) . .
F4 B1 F1 107.6(6) 2_655 .
F3 B1 F2 105.6(7) . .
F4 B1 F2 105.4(8) . .
F1 B1 F2 103.6(4) . .
F3 B1 F2 105.6(7) 2_655 2_655
F4 B1 F2 105.4(8) 2_655 2_655
F1 B1 F2 103.6(4) . 2_655
F2 B1 F2 152.7(8) . 2_655
B1 F1 Cr3 180.000(1) . .
C1 N1 C5 117.6(2) . .
C1 N1 Cr1 118.4(2) . .
C5 N1 Cr1 123.8(2) . .
C10 N2 C5 122.0(2) . .
C10 N2 Cr2 115.2(2) . .
C5 N2 Cr2 122.8(2) . .
C10 N3 C6 119.3(2) . .
C10 N3 Cr3 117.5(2) . .
C6 N3 Cr3 122.8(2) . .
C11 N4 C15 117.9(3) . .
C11 N4 Cr1 118.7(2) . .
C15 N4 Cr1 123.2(2) . .
C20 N5 C15 121.3(2) . .
C20 N5 Cr2 115.6(2) . .
C15 N5 Cr2 122.8(2) . .
C16 N6 C20 118.7(2) . .
C16 N6 Cr3 123.4(2) . .
C20 N6 Cr3 118.0(2) . .
N1 C1 C2 123.8(3) . .
N1 C1 H1 113.1(20) . .
C2 C1 H1 123.1(20) . .
C1 C2 C3 118.4(3) . .
C1 C2 H2 119.3(21) . .
C3 C2 H2 122.1(20) . .
C4 C3 C2 119.3(3) . .
C4 C3 H3 119.7(21) . .
C2 C3 H3 120.8(21) . .
C3 C4 C5 120.1(3) . .
C3 C4 H4 121.7(19) . .
C5 C4 H4 118.2(19) . .
N1 C5 N2 116.0(2) . .
N1 C5 C4 120.3(3) . .
N2 C5 C4 123.6(3) . .
N3 C6 C7 122.9(3) . .
N3 C6 H6 112.4(21) . .
C7 C6 H6 124.7(21) . .
C6 C7 C8 118.2(3) . .
C6 C7 H8 118.9(22) . .
C8 C7 H8 122.9(22) . .
C9 C8 C7 120.1(3) . .
C9 C8 H8 122.6(20) . .
C7 C8 H8 117.3(20) . .
C8 C9 C10 119.9(3) . .
C8 C9 H9 119.5(18) . .
C10 C9 H9 120.6(18) . .
N3 C10 N2 113.9(2) . .
N3 C10 C9 119.4(3) . .
N2 C10 C9 126.5(3) . .
N4 C11 C12 124.0(3) . .
N4 C11 H11 114.8(19) . .
C12 C11 H11 121.2(19) . .
C11 C12 C13 118.2(3) . .
C11 C12 H12 120.7(24) . .
C13 C12 H12 121.1(24) . .
C14 C13 C12 119.3(3) . .
C14 C13 H13 119.0(20) . .
C12 C13 H13 121.7(20) . .
C13 C14 C15 120.3(3) . .
C13 C14 H14 121.2(20) . .
C15 C14 H14 118.5(20) . .
N4 C15 N5 116.0(2) . .
N4 C15 C14 120.0(3) . .
N5 C15 C14 123.8(3) . .
C17 C16 N6 123.0(3) . .
C17 C16 H16 121.2(18) . .
N6 C16 H16 115.8(18) . .
C16 C17 C18 118.9(3) . .
C16 C17 H17 119.0(22) . .
C18 C17 H17 122.0(22) . .
C19 C18 C17 119.5(3) . .
C19 C18 H18 118.1(19) . .
C17 C18 H18 122.4(19) . .
C18 C19 C20 119.8(3) . .
C18 C19 H19 119.9(20) . .
C20 C19 H19 120.1(21) . .
N6 C20 N5 114.2(2) . .
N6 C20 C19 120.0(3) . .
N5 C20 C19 125.7(3) . .
Cl3 C21 Cl2 112.4(3) . .
Cl3 C21 Cl3A 34.7(4) . .
Cl2 C21 Cl3A 107.9(3) . .
Cl3 C21 H21A 125.3(36) . .
Cl2 C21 H21A 104.8(35) . .
Cl3A C21 H21A 96.9(36) . .
Cl3 C21 H22A 85.9(25) . .
Cl2 C21 H22A 117.0(24) . .
Cl3A C21 H22A 116.6(25) . .
H21A C21 H22A 111.2(42) . .
Cl3 Cl3A C21 69.3(4) . .
Cl3A Cl3 C21 76.0(7) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Cr1 N4 2.135(2) y
Cr1 N1 2.161(2) y
Cr1 Cl1 2.5299(11) y
Cr1 Cr2 2.6427(8) y
Cr2 Cr3 1.9952(8) y
Cr2 N5 2.029(2) y
Cr2 N2 2.029(2) y
Cr3 N3 2.075(2) y
Cr3 N6 2.084(2) y
Cr3 F1 2.374(3) y
B1 F3 1.269(8) ?
B1 F4 1.304(10) ?
B1 F1 1.378(7) ?
B1 F2 1.459(7) ?
N1 C1 1.357(4) ?
N1 C5 1.364(4) ?
N2 C10 1.377(4) ?
N2 C5 1.381(4) ?
N3 C10 1.361(4) ?
N3 C6 1.362(4) ?
N4 C11 1.358(4) ?
N4 C15 1.361(4) ?
N5 C20 1.378(4) ?
N5 C15 1.384(4) ?
N6 C16 1.358(4) ?
N6 C20 1.367(4) ?
C1 C2 1.372(5) ?
C1 H1 0.89(3) ?
C2 C3 1.383(5) ?
C2 H2 0.91(3) ?
C3 C4 1.370(5) ?
C3 H3 0.90(4) ?
C4 C5 1.409(4) ?
C4 H4 0.91(3) ?
C6 C7 1.363(5) ?
C6 H6 0.91(4) ?
C7 C8 1.390(5) ?
C7 H8 0.87(4) ?
C8 C9 1.367(4) ?
C8 H8 0.90(4) ?
C9 C10 1.409(4) ?
C9 H9 0.93(3) ?
C11 C12 1.368(5) ?
C11 H11 0.88(3) ?
C12 C13 1.386(5) ?
C12 H12 0.94(4) ?
C13 C14 1.371(5) ?
C13 H13 0.96(4) ?
C14 C15 1.409(4) ?
C14 H14 0.89(3) ?
C16 C17 1.358(4) ?
C16 H16 0.90(3) ?
C17 C18 1.385(5) ?
C17 H17 0.85(4) ?
C18 C19 1.377(5) ?
C18 H18 0.93(3) ?
C19 C20 1.401(4) ?
C19 H19 0.90(3) ?
C21 Cl3 1.734(8) ?
C21 Cl2 1.757(4) ?
C21 Cl3A 1.799(6) ?
C21 H21A 0.87(6) ?
C21 H22A 0.96(4) ?
loop_
_cod_changelog_entry_id
_cod_changelog_entry_author
_cod_changelog_entry_date
_cod_changelog_entry_text
1 'Vaitkus, Antanas' 2021-10-29T14:40:00+03:00
'Updated bibliographic information.'
