#------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/51/54/1515491.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_1515491
loop_
_publ_author_name
'Cho, Jaeheung'
'Woo, Jaeyoung'
'Eun Han, Jung'
'Kubo, Minoru'
'Ogura, Takashi'
'Nam, Wonwoo'
_publ_section_title
;
 Chromium(v)-oxo and chromium(iii)-superoxo complexes bearing a
 macrocyclic TMC ligand in hydrogen atom abstraction reactions
;
_journal_issue                   10
_journal_name_full               'Chemical Science'
_journal_page_first              2057
_journal_paper_doi               10.1039/c1sc00386k
_journal_volume                  2
_journal_year                    2011
_chemical_formula_sum            'C15 H35 Cl2 Cr N4 O10'
_chemical_formula_weight         554.37
_chemical_name_systematic
;
?
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.2150(4)
_cell_length_b                   9.7664(3)
_cell_length_c                   16.4588(5)
_cell_measurement_reflns_used    9941
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.17
_cell_measurement_theta_min      2.42
_cell_volume                     2284.96(12)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and 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  0.0329
_diffrn_reflns_av_sigmaI/netI    0.0128
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            34238
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.89
_exptl_absorpt_coefficient_mu    0.794
_exptl_absorpt_correction_T_max  0.9248
_exptl_absorpt_correction_T_min  0.8574
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.611
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needle
_exptl_crystal_F_000             1164
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.847
_refine_diff_density_min         -0.722
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.164
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         2378
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.164
_refine_ls_R_factor_all          0.0531
_refine_ls_R_factor_gt           0.0486
_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)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2021
_refine_ls_wR_factor_ref         0.2095
_reflns_number_gt                2117
_reflns_number_total             2378
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1sc00386k.txt
_cod_data_source_block           chem084
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      Pnma
_cod_database_code               1515491
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Cr1 Cr 0.73290(4) 0.2500 0.40402(4) 0.0125(3) Uani 1 2 d S
Cl1 Cl 0.02059(7) 0.2500 0.71890(6) 0.0194(3) Uani 1 2 d S
Cl2 Cl 0.31723(7) 0.2500 0.39518(6) 0.0185(3) Uani 1 2 d S
O1 O 0.79149(19) 0.2500 0.32072(17) 0.0176(6) Uani 1 2 d S
O2 O 0.66549(18) 0.2500 0.49407(17) 0.0186(7) Uani 1 2 d S
N2 N 0.82326(15) 0.0908(3) 0.44886(14) 0.0178(6) Uani 1 1 d .
N1 N 0.65560(16) 0.0852(2) 0.35291(14) 0.0167(5) Uani 1 1 d .
C1 C 0.9648(3) 0.2500 0.4426(3) 0.0227(10) Uani 1 2 d S
H1A H 1.0293 0.2500 0.4233 0.027 Uiso 1 2 calc SR
H1B H 0.9674 0.2500 0.5015 0.027 Uiso 1 2 calc SR
C4 C 0.72983(19) -0.0201(3) 0.33886(19) 0.0203(7) Uani 1 1 d .
H4A H 0.7714 0.0098 0.2956 0.024 Uiso 1 1 calc R
H4B H 0.7008 -0.1056 0.3223 0.024 Uiso 1 1 calc R
C6 C 0.5550(3) 0.2500 0.2713(3) 0.0258(10) Uani 1 2 d S
H6A H 0.5141 0.2500 0.3186 0.031 Uiso 1 2 calc SR
H6B H 0.5152 0.2500 0.2234 0.031 Uiso 1 2 calc SR
C3 C 0.7854(2) -0.0419(3) 0.41512(19) 0.0215(7) Uani 1 1 d .
H3A H 0.8375 -0.1032 0.4038 0.026 Uiso 1 1 calc R
H3B H 0.7456 -0.0851 0.4556 0.026 Uiso 1 1 calc R
C2 C 0.92018(19) 0.1159(3) 0.41630(18) 0.0204(7) Uani 1 1 d .
H2A H 0.9174 0.1141 0.3574 0.024 Uiso 1 1 calc R
H2B H 0.9606 0.0413 0.4334 0.024 Uiso 1 1 calc R
C5 C 0.6132(2) 0.1199(3) 0.27184(17) 0.0213(7) Uani 1 1 d .
H5A H 0.5737 0.0443 0.2546 0.026 Uiso 1 1 calc R
H5B H 0.6635 0.1291 0.2324 0.026 Uiso 1 1 calc R
O6 O 0.2172(2) 0.2500 0.40935(19) 0.0236(8) Uani 1 2 d S
O8 O 0.3657(2) 0.2500 0.47222(19) 0.0285(8) Uani 1 2 d S
O3 O -0.0681(4) 0.2500 0.7567(4) 0.082(2) Uani 1 2 d S
O4 O 0.0175(3) 0.2500 0.6316(3) 0.0473(10) Uani 1 2 d S
O7 O 0.34284(16) 0.1289(2) 0.35082(14) 0.0298(6) Uani 1 1 d .
O5 O 0.0685(2) 0.1284(3) 0.74651(18) 0.0474(8) Uani 1 1 d .
C8 C 0.5802(2) 0.0305(3) 0.40626(18) 0.0225(7) Uani 1 1 d .
H8A H 0.5523 -0.0485 0.3812 0.034 Uiso 1 1 calc R
H8B H 0.5329 0.0994 0.4142 0.034 Uiso 1 1 calc R
H8C H 0.6065 0.0051 0.4578 0.034 Uiso 1 1 calc R
C7 C 0.8280(2) 0.0724(4) 0.53913(18) 0.0234(7) Uani 1 1 d .
H7A H 0.7655 0.0666 0.5608 0.035 Uiso 1 1 calc R
H7B H 0.8600 0.1490 0.5630 0.035 Uiso 1 1 calc R
H7C H 0.8617 -0.0103 0.5515 0.035 Uiso 1 1 calc R
C9 C 0.6070(3) 0.2500 0.5630(3) 0.0302(11) Uani 1 2 d S
H9A H 0.5433 0.2675 0.5468 0.045 Uiso 0.50 1 calc PR
H9B H 0.6273 0.3201 0.6000 0.045 Uiso 0.50 1 calc PR
H9C H 0.6106 0.1624 0.5894 0.045 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 O2 178.39(13) . .
O1 Cr1 N1 85.99(9) . 7_565
O2 Cr1 N1 92.97(9) . 7_565
O1 Cr1 N1 85.99(9) . .
O2 Cr1 N1 92.97(9) . .
N1 Cr1 N1 98.61(12) 7_565 .
O1 Cr1 N2 89.03(9) . .
O2 Cr1 N2 92.07(9) . .
N1 Cr1 N2 174.15(9) 7_565 .
N1 Cr1 N2 84.09(9) . .
O1 Cr1 N2 89.03(9) . 7_565
O2 Cr1 N2 92.07(9) . 7_565
N1 Cr1 N2 84.09(9) 7_565 7_565
N1 Cr1 N2 174.15(9) . 7_565
N2 Cr1 N2 92.77(13) . 7_565
O3 Cl1 O4 114.5(3) . .
O3 Cl1 O5 106.49(19) . .
O4 Cl1 O5 109.24(14) . .
O3 Cl1 O5 106.50(19) . 7_565
O4 Cl1 O5 109.23(14) . 7_565
O5 Cl1 O5 110.8(2) . 7_565
O7 Cl2 O7 110.8(2) 7_565 .
O7 Cl2 O6 109.40(12) 7_565 .
O7 Cl2 O6 109.40(12) . .
O7 Cl2 O8 109.00(12) 7_565 .
O7 Cl2 O8 108.99(12) . .
O6 Cl2 O8 109.23(19) . .
C9 O2 Cr1 176.7(3) . .
C7 N2 C2 109.4(2) . .
C7 N2 C3 106.1(2) . .
C2 N2 C3 109.7(2) . .
C7 N2 Cr1 117.06(18) . .
C2 N2 Cr1 107.98(17) . .
C3 N2 Cr1 106.38(16) . .
C8 N1 C4 110.7(2) . .
C8 N1 C5 108.4(2) . .
C4 N1 C5 107.5(2) . .
C8 N1 Cr1 114.35(18) . .
C4 N1 Cr1 102.60(16) . .
C5 N1 Cr1 112.90(18) . .
C2 C1 C2 119.2(3) . 7_565
N1 C4 C3 109.9(2) . .
C5 C6 C5 113.8(3) . 7_565
C4 C3 N2 112.0(2) . .
N2 C2 C1 115.0(3) . .
N1 C5 C6 114.3(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cr1 O1 1.604(3) .
Cr1 O2 1.765(3) .
Cr1 N1 2.122(2) 7_565
Cr1 N1 2.122(2) .
Cr1 N2 2.148(2) .
Cr1 N2 2.148(2) 7_565
Cl1 O3 1.407(4) .
Cl1 O4 1.437(4) .
Cl1 O5 1.442(3) .
Cl1 O5 1.442(3) 7_565
Cl2 O7 1.437(2) 7_565
Cl2 O7 1.437(2) .
Cl2 O6 1.441(3) .
Cl2 O8 1.443(3) .
O2 C9 1.407(5) .
N2 C7 1.498(4) .
N2 C2 1.498(3) .
N2 C3 1.509(4) .
N1 C8 1.485(4) .
N1 C4 1.492(4) .
N1 C5 1.503(3) .
C1 C2 1.518(4) .
C1 C2 1.519(4) 7_565
C4 C3 1.498(4) .
C6 C5 1.517(4) .
C6 C5 1.517(4) 7_565
