#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:26:45 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179246 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/66/4316615.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_4316615
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         'C9 H9 Cr N O7'
_chemical_formula_sum            'C9 H9 Cr N O7'
_chemical_formula_weight         295.17
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 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                 115.838(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.8978(12)
_cell_length_b                   15.4219(14)
_cell_length_c                   6.8108(6)
_cell_measurement_reflns_used    5563
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      30.01
_cell_measurement_theta_min      2.20
_cell_volume                     1219.29(19)
_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, 1997)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0145
_diffrn_reflns_av_sigmaI/netI    0.0301
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            6761
_diffrn_reflns_theta_full        30.01
_diffrn_reflns_theta_max         30.01
_diffrn_reflns_theta_min         2.20
_exptl_absorpt_coefficient_mu    0.963
_exptl_absorpt_correction_T_max  0.742
_exptl_absorpt_correction_T_min  0.643
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2.03; (Sheldrick)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.608
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             600
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.31
_refine_diff_density_max         0.294
_refine_diff_density_min         -0.159
_refine_diff_density_rms         0.046
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.023(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         3393
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0195
_refine_ls_R_factor_gt           0.0193
_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)+(0.0247P)²+0.0942P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0506
_refine_ls_wR_factor_ref         0.0507
_reflns_number_gt                3360
_reflns_number_total             3393
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic101230j_si_002_2.cif
_cod_data_source_block           Complex_1-Cr-a
_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_database_code               4316615
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'
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 -0.05416(11) 0.22922(8) 0.6894(2) 0.0195(2) Uani 1 1 d . . .
C2 C 0.14338(11) 0.27047(8) 0.7095(2) 0.0199(2) Uani 1 1 d . . .
C3 C 0.12477(11) 0.14085(9) 0.9638(2) 0.0178(2) Uani 1 1 d . . .
C4 C -0.03399(12) 0.06424(9) 0.6201(2) 0.0209(2) Uani 1 1 d . . .
C5 C -0.01641(11) 0.18267(9) 0.3504(2) 0.0182(2) Uani 1 1 d . . .
C6 C 0.30066(10) 0.13146(8) 0.6600(2) 0.0165(2) Uani 1 1 d . . .
H6A H 0.3405 0.1483 0.8156 0.020 Uiso 1 1 calc R . .
H6B H 0.2840 0.1851 0.5715 0.020 Uiso 1 1 calc R . .
C7 C 0.37952(10) 0.07442(8) 0.60503(19) 0.0161(2) Uani 1 1 d . . .
C8 C 0.56463(11) 0.06536(10) 0.6141(2) 0.0248(3) Uani 1 1 d . . .
H8A H 0.5354 0.0700 0.4539 0.030 Uiso 1 1 calc R . .
H8B H 0.5729 0.0032 0.6542 0.030 Uiso 1 1 calc R . .
C9 C 0.67810(13) 0.11035(13) 0.7258(3) 0.0344(3) Uani 1 1 d . . .
H9A H 0.6691 0.1716 0.6833 0.052 Uiso 1 1 calc R . .
H9B H 0.7339 0.0831 0.6832 0.052 Uiso 1 1 calc R . .
H9C H 0.7058 0.1058 0.8842 0.052 Uiso 1 1 calc R . .
Cr1 Cr 0.059161(15) 0.164103(11) 0.660493(18) 0.01432(5) Uani 1 1 d . . .
N1 N 0.19157(9) 0.08855(7) 0.61967(18) 0.01582(19) Uani 1 1 d . . .
H1A H 0.1613(15) 0.0687(12) 0.488(3) 0.023(4) Uiso 1 1 d . . .
H1B H 0.2096(15) 0.0447(13) 0.703(3) 0.020(4) Uiso 1 1 d . . .
O1 O -0.12347(9) 0.27106(7) 0.70659(17) 0.0287(2) Uani 1 1 d . . .
O2 O 0.18705(11) 0.33693(6) 0.74389(19) 0.0305(2) Uani 1 1 d . . .
O3 O 0.15623(9) 0.12616(7) 1.14533(16) 0.0250(2) Uani 1 1 d . . .
O4 O -0.09352(10) 0.00653(8) 0.6012(2) 0.0342(3) Uani 1 1 d . . .
O5 O -0.06658(9) 0.19264(7) 0.16720(16) 0.0255(2) Uani 1 1 d . . .
O6 O 0.34945(8) 0.00848(6) 0.49844(16) 0.02246(18) Uani 1 1 d . . .
O7 O 0.48540(8) 0.10710(6) 0.68410(16) 0.02037(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 178.64(11) . . ?
O2 C2 Cr1 174.26(12) . . ?
O3 C3 Cr1 174.91(12) . . ?
O4 C4 Cr1 176.06(13) . . ?
O5 C5 Cr1 176.33(12) . . ?
N1 C6 C7 112.65(10) . . ?
N1 C6 H6A 109.1 . . ?
C7 C6 H6A 109.1 . . ?
N1 C6 H6B 109.1 . . ?
C7 C6 H6B 109.1 . . ?
H6A C6 H6B 107.8 . . ?
O6 C7 O7 124.42(11) . . ?
O6 C7 C6 124.30(11) . . ?
O7 C7 C6 111.26(10) . . ?
O7 C8 C9 107.48(12) . . ?
O7 C8 H8A 110.2 . . ?
C9 C8 H8A 110.2 . . ?
O7 C8 H8B 110.2 . . ?
C9 C8 H8B 110.2 . . ?
H8A C8 H8B 108.5 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C1 Cr1 C3 89.14(6) . . ?
C1 Cr1 C4 88.65(6) . . ?
C3 Cr1 C4 87.61(6) . . ?
C1 Cr1 C2 86.04(6) . . ?
C3 Cr1 C2 91.26(6) . . ?
C4 Cr1 C2 174.59(6) . . ?
C1 Cr1 C5 89.44(5) . . ?
C3 Cr1 C5 175.99(6) . . ?
C4 Cr1 C5 88.61(6) . . ?
C2 Cr1 C5 92.38(6) . . ?
C1 Cr1 N1 178.80(5) . . ?
C3 Cr1 N1 92.03(5) . . ?
C4 Cr1 N1 91.68(5) . . ?
C2 Cr1 N1 93.65(5) . . ?
C5 Cr1 N1 89.42(5) . . ?
C6 N1 Cr1 118.34(7) . . ?
C6 N1 H1A 108.5(12) . . ?
Cr1 N1 H1A 107.2(12) . . ?
C6 N1 H1B 105.9(12) . . ?
Cr1 N1 H1B 110.2(12) . . ?
H1A N1 H1B 106.1(17) . . ?
C7 O7 C8 116.38(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 1.1491(16) . ?
C1 Cr1 1.8531(13) . ?
C2 O2 1.1435(17) . ?
C2 Cr1 1.9147(13) . ?
C3 O3 1.1437(17) . ?
C3 Cr1 1.8940(13) . ?
C4 O4 1.1455(18) . ?
C4 Cr1 1.8982(14) . ?
C5 O5 1.1383(17) . ?
C5 Cr1 1.9230(13) . ?
C6 N1 1.4684(16) . ?
C6 C7 1.5102(17) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 O6 1.2108(15) . ?
C7 O7 1.3295(15) . ?
C8 O7 1.4527(15) . ?
C8 C9 1.494(2) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
Cr1 N1 2.1829(11) . ?
N1 H1A 0.862(19) . ?
N1 H1B 0.85(2) . ?
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 H1A O3 0.862(19) 2.472(19) 3.1141(15) 131.8(15) 1_554
N1 H1B O6 0.85(2) 2.195(18) 2.9089(14) 142.0(16) 2
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 O6 14.52(17) . . . . ?
N1 C6 C7 O7 -167.05(10) . . . . ?
C7 C6 N1 Cr1 -174.51(8) . . . . ?
C3 Cr1 N1 C6 -85.33(9) . . . . ?
C4 Cr1 N1 C6 -173.00(9) . . . . ?
C2 Cr1 N1 C6 6.07(9) . . . . ?
C5 Cr1 N1 C6 98.42(9) . . . . ?
O6 C7 O7 C8 7.50(18) . . . . ?
C6 C7 O7 C8 -170.93(11) . . . . ?
C9 C8 O7 C7 -178.51(12) . . . . ?
