#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:26:45 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179246 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/66/4316620.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_4316620
loop_
_publ_author_name
'Wei-Qiang Zhang'
'Adrian C. Whitwood'
'Ian J. S. Fairlamb'
'Jason M. Lynam'
_publ_contact_author_address
;Department of Chemistry
University of York
Heslington
York
YO10 5DD
UK        
;
_publ_contact_author_email       jml12@york.ac.uk
_publ_contact_author_fax         +44(0)1904432516
_publ_contact_author_name        'Jason M Lynam'
_publ_contact_author_phone       +44(0)1904432534
_publ_section_title
;
 Group 6 Carbon Monoxide-Releasing Metal Complexes with
 Biologically-Compatible Leaving Groups
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8941
_journal_page_last               8952
_journal_paper_doi               10.1021/ic101230j
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C16 H13 Cr N O7'
_chemical_formula_sum            'C16 H13 Cr N O7'
_chemical_formula_weight         383.27
_chemical_name_systematic
; 
 ? 
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 118.841(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   23.559(2)
_cell_length_b                   7.6899(6)
_cell_length_c                   21.4427(18)
_cell_measurement_reflns_used    9061
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      30.01
_cell_measurement_theta_min      2.83
_cell_volume                     3402.8(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0170
_diffrn_reflns_av_sigmaI/netI    0.0154
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            18543
_diffrn_reflns_theta_full        30.02
_diffrn_reflns_theta_max         30.02
_diffrn_reflns_theta_min         1.97
_exptl_absorpt_coefficient_mu    0.710
_exptl_absorpt_correction_T_max  0.952
_exptl_absorpt_correction_T_min  0.796
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2.10; (Sheldrick)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.496
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.492
_refine_diff_density_min         -0.302
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     239
_refine_ls_number_reflns         4889
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0336
_refine_ls_R_factor_gt           0.0295
_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)+(0.0470P)²+2.2926P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0785
_refine_ls_wR_factor_ref         0.0816
_reflns_number_gt                4368
_reflns_number_total             4889
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic101230j_si_002_7.cif
_cod_data_source_block           Complex_3b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        3402.9(5)
_cod_database_code               4316620
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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.18392(6) -0.09198(15) 0.45833(6) 0.0202(2) Uani 1 1 d . . .
C2 C 0.07138(6) 0.03156(17) 0.35573(7) 0.0260(3) Uani 1 1 d . . .
C3 C 0.24291(6) -0.00774(14) 0.38341(6) 0.0192(2) Uani 1 1 d . . .
C4 C 0.13380(6) -0.20837(16) 0.32659(6) 0.0215(2) Uani 1 1 d . . .
C5 C 0.17564(6) 0.23733(16) 0.41394(6) 0.0215(2) Uani 1 1 d . . .
C6 C 0.12980(5) 0.13093(14) 0.27154(6) 0.0167(2) Uani 1 1 d . . .
C7 C 0.15084(5) 0.05562(14) 0.22156(6) 0.0171(2) Uani 1 1 d . . .
C8 C 0.11834(6) -0.08792(15) 0.17926(6) 0.0198(2) Uani 1 1 d . . .
H8 H 0.0828 -0.1373 0.1823 0.024 Uiso 1 1 calc R . .
C9 C 0.13775(6) -0.15900(16) 0.13275(6) 0.0231(2) Uani 1 1 d . . .
H9 H 0.1151 -0.2558 0.1039 0.028 Uiso 1 1 calc R . .
C10 C 0.19001(6) -0.08884(17) 0.12850(7) 0.0253(2) Uani 1 1 d . . .
H10 H 0.2033 -0.1374 0.0968 0.030 Uiso 1 1 calc R . .
C11 C 0.22285(6) 0.05260(18) 0.17069(7) 0.0259(2) Uani 1 1 d . . .
H11 H 0.2588 0.1003 0.1679 0.031 Uiso 1 1 calc R . .
C12 C 0.20367(6) 0.12519(16) 0.21703(6) 0.0222(2) Uani 1 1 d . . .
H12 H 0.2265 0.2221 0.2457 0.027 Uiso 1 1 calc R . .
C13 C 0.08194(6) 0.37236(16) 0.18478(6) 0.0214(2) Uani 1 1 d . . .
C14 C 0.01461(6) 0.45006(15) 0.15091(6) 0.0197(2) Uani 1 1 d . . .
C15 C -0.05671(6) 0.62950(18) 0.05413(7) 0.0276(3) Uani 1 1 d . . .
H15A H -0.0712 0.6892 0.0849 0.033 Uiso 1 1 calc R . .
H15B H -0.0888 0.5385 0.0265 0.033 Uiso 1 1 calc R . .
C16 C -0.05026(7) 0.7576(2) 0.00486(7) 0.0334(3) Uani 1 1 d . . .
H16A H -0.0216 0.8528 0.0328 0.050 Uiso 1 1 calc R . .
H16B H -0.0930 0.8045 -0.0283 0.050 Uiso 1 1 calc R . .
H16C H -0.0319 0.6989 -0.0220 0.050 Uiso 1 1 calc R . .
Cr1 Cr 0.156456(8) 0.01394(2) 0.369349(9) 0.01535(6) Uani 1 1 d . . .
H1 H 0.0843(8) 0.324(2) 0.2769(9) 0.030(4) Uiso 1 1 d . . .
H13A H 0.1145(8) 0.464(2) 0.1947(9) 0.021(4) Uiso 1 1 d . . .
H13B H 0.0827(8) 0.298(2) 0.1506(9) 0.032(4) Uiso 1 1 d . . .
N1 N 0.09715(5) 0.27675(13) 0.24991(5) 0.01876(18) Uani 1 1 d . . .
O1 O 0.19992(5) -0.15761(13) 0.51221(5) 0.02765(19) Uani 1 1 d . . .
O2 O 0.02036(5) 0.03630(17) 0.34920(8) 0.0497(3) Uani 1 1 d . . .
O3 O 0.29478(5) -0.02237(12) 0.39317(6) 0.0273(2) Uani 1 1 d . . .
O4 O 0.11922(5) -0.34504(12) 0.30312(6) 0.0323(2) Uani 1 1 d . . .
O5 O 0.18649(5) 0.36880(13) 0.44168(6) 0.0354(2) Uani 1 1 d . . .
O6 O -0.02593(5) 0.42339(13) 0.16841(5) 0.0292(2) Uani 1 1 d . . .
O7 O 0.00729(4) 0.55237(12) 0.09726(5) 0.02315(18) Uani 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'
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'
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
_geom_angle_publ_flag
O1 C1 Cr1 179.12(11) . . ?
O2 C2 Cr1 177.18(12) . . ?
O3 C3 Cr1 178.51(11) . . ?
O4 C4 Cr1 176.68(11) . . ?
O5 C5 Cr1 178.20(12) . . ?
N1 C6 C7 114.69(10) . . ?
N1 C6 Cr1 124.50(8) . . ?
C7 C6 Cr1 120.72(8) . . ?
C8 C7 C12 118.89(10) . . ?
C8 C7 C6 120.18(10) . . ?
C12 C7 C6 120.92(10) . . ?
C9 C8 C7 120.50(11) . . ?
C9 C8 H8 119.8 . . ?
C7 C8 H8 119.8 . . ?
C10 C9 C8 120.17(12) . . ?
C10 C9 H9 119.9 . . ?
C8 C9 H9 119.9 . . ?
C9 C10 C11 119.71(11) . . ?
C9 C10 H10 120.1 . . ?
C11 C10 H10 120.1 . . ?
C10 C11 C12 120.61(11) . . ?
C10 C11 H11 119.7 . . ?
C12 C11 H11 119.7 . . ?
C11 C12 C7 120.12(11) . . ?
C11 C12 H12 119.9 . . ?
C7 C12 H12 119.9 . . ?
N1 C13 C14 111.99(10) . . ?
N1 C13 H13A 110.2(9) . . ?
C14 C13 H13A 110.3(9) . . ?
N1 C13 H13B 110.7(11) . . ?
C14 C13 H13B 106.1(10) . . ?
H13A C13 H13B 107.4(14) . . ?
O6 C14 O7 125.37(11) . . ?
O6 C14 C13 126.19(11) . . ?
O7 C14 C13 108.43(10) . . ?
O7 C15 C16 106.68(11) . . ?
O7 C15 H15A 110.4 . . ?
C16 C15 H15A 110.4 . . ?
O7 C15 H15B 110.4 . . ?
C16 C15 H15B 110.4 . . ?
H15A C15 H15B 108.6 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C1 Cr1 C2 90.46(5) . . ?
C1 Cr1 C4 88.79(5) . . ?
C2 Cr1 C4 87.68(6) . . ?
C1 Cr1 C5 89.95(5) . . ?
C2 Cr1 C5 89.43(6) . . ?
C4 Cr1 C5 176.84(5) . . ?
C1 Cr1 C3 89.04(5) . . ?
C2 Cr1 C3 179.12(5) . . ?
C4 Cr1 C3 91.58(5) . . ?
C5 Cr1 C3 91.29(5) . . ?
C1 Cr1 C6 177.73(5) . . ?
C2 Cr1 C6 91.80(5) . . ?
C4 Cr1 C6 91.42(5) . . ?
C5 Cr1 C6 89.96(5) . . ?
C3 Cr1 C6 88.70(5) . . ?
C6 N1 C13 126.85(10) . . ?
C6 N1 H1 117.7(12) . . ?
C13 N1 H1 115.4(12) . . ?
C14 O7 C15 116.71(10) . . ?
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
C1 O1 1.1452(15) . ?
C1 Cr1 1.8792(12) . ?
C2 O2 1.1416(17) . ?
C2 Cr1 1.8859(13) . ?
C3 O3 1.1416(16) . ?
C3 Cr1 1.9170(13) . ?
C4 O4 1.1441(15) . ?
C4 Cr1 1.8911(13) . ?
C5 O5 1.1377(15) . ?
C5 Cr1 1.9112(12) . ?
C6 N1 1.3115(14) . ?
C6 C7 1.4973(15) . ?
C6 Cr1 2.0813(11) . ?
C7 C8 1.3991(16) . ?
C7 C12 1.4005(16) . ?
C8 C9 1.3937(16) . ?
C8 H8 0.9500 . ?
C9 C10 1.3868(18) . ?
C9 H9 0.9500 . ?
C10 C11 1.387(2) . ?
C10 H10 0.9500 . ?
C11 C12 1.3916(17) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 N1 1.4616(14) . ?
C13 C14 1.5130(16) . ?
C13 H13A 0.987(17) . ?
C13 H13B 0.937(18) . ?
C14 O6 1.2003(15) . ?
C14 O7 1.3345(14) . ?
C15 O7 1.4614(14) . ?
C15 C16 1.5049(19) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
N1 H1 0.853(17) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1 O6 0.853(17) 2.325(17) 3.1608(14) 166.3(16) 2
N1 H1 O4 0.853(17) 2.648(18) 3.0755(14) 112.3(13) 1_565
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 C6 C7 C8 -104.08(12) . . . . ?
Cr1 C6 C7 C8 79.16(12) . . . . ?
N1 C6 C7 C12 76.90(14) . . . . ?
Cr1 C6 C7 C12 -99.86(11) . . . . ?
C12 C7 C8 C9 -0.80(17) . . . . ?
C6 C7 C8 C9 -179.83(10) . . . . ?
C7 C8 C9 C10 0.62(18) . . . . ?
C8 C9 C10 C11 -0.08(19) . . . . ?
C9 C10 C11 C12 -0.26(19) . . . . ?
C10 C11 C12 C7 0.07(19) . . . . ?
C8 C7 C12 C11 0.45(17) . . . . ?
C6 C7 C12 C11 179.48(11) . . . . ?
N1 C13 C14 O6 -8.38(18) . . . . ?
N1 C13 C14 O7 172.42(10) . . . . ?
N1 C6 Cr1 C2 49.75(10) . . . . ?
C7 C6 Cr1 C2 -133.82(9) . . . . ?
N1 C6 Cr1 C4 137.48(10) . . . . ?
C7 C6 Cr1 C4 -46.09(9) . . . . ?
N1 C6 Cr1 C5 -39.68(10) . . . . ?
C7 C6 Cr1 C5 136.75(9) . . . . ?
N1 C6 Cr1 C3 -130.97(10) . . . . ?
C7 C6 Cr1 C3 45.46(9) . . . . ?
C7 C6 N1 C13 -2.27(16) . . . . ?
Cr1 C6 N1 C13 174.36(9) . . . . ?
C14 C13 N1 C6 141.80(11) . . . . ?
O6 C14 O7 C15 -3.74(18) . . . . ?
C13 C14 O7 C15 175.47(10) . . . . ?
C16 C15 O7 C14 171.99(11) . . . . ?
