#------------------------------------------------------------------------------
#$Date: 2015-12-09 16:29:51 +0200 (Wed, 09 Dec 2015) $
#$Revision: 171207 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/67/7036792.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_7036792
loop_
_publ_author_name
'Chan, Chung Ying'
'Barnard, Peter J.'
_publ_section_title
;
 Rhenium complexes of bidentate, bis-bidentate and tridentate
 N-heterocyclic carbene ligands.
;
_journal_issue                   44
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              19126
_journal_page_last               19140
_journal_paper_doi               10.1039/c5dt03295d
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C12 H12 Cl N4 O3 Re'
_chemical_formula_sum            'C12 H12 Cl N4 O3 Re'
_chemical_formula_weight         481.91
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-07-08
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-08-20 deposited with the CCDC.
2015-10-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.879(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.6760(3)
_cell_length_b                   17.0407(7)
_cell_length_c                   11.3204(5)
_cell_measurement_temperature    150
_cell_volume                     1479.96(11)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0293
_diffrn_reflns_av_unetI/netI     0.0343
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            7793
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.369
_diffrn_reflns_theta_min         2.912
_exptl_absorpt_coefficient_mu    8.405
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73977
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.163
_exptl_crystal_description       block
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.201
_refine_diff_density_min         -0.878
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     192
_refine_ls_number_reflns         3031
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0240
_refine_ls_R_factor_gt           0.0196
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[σ²(Fo²)+(0.0114P)²]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0383
_refine_ls_wR_factor_ref         0.0399
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2717
_reflns_number_total             3031
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5dt03295d2.cif
_cod_data_source_block           14
_cod_depositor_comments
'Adding full bibliography for 7036787--7036794.cif.'
_cod_original_cell_volume        1479.97(11)
_cod_database_code               7036792
_shelxl_version_number           2013-2
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C5(H5), C10(H10), C9(H9)
2.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C11(H11A,H11B,H11C)
;
_olex2_date_sample_data_collection 2014-07-11
_olex2_submission_original_sample_id PJB290
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
Re1 Re 0.22643(2) 0.41855(2) 0.19506(2) 0.01586(5) Uani 1 1 d .
Cl1 Cl 0.08123(9) 0.39808(5) 0.38935(8) 0.02365(18) Uani 1 1 d .
C2 C 0.0617(4) 0.3460(2) 0.1193(3) 0.0253(8) Uani 1 1 d .
N1 N 0.5826(3) 0.48107(14) 0.3007(3) 0.0179(6) Uani 1 1 d .
C6 C 0.5445(4) 0.58286(18) 0.4106(3) 0.0273(8) Uani 1 1 d .
H6 H 0.5622 0.6262 0.4624 0.033 Uiso 1 1 calc R
C8 C 0.4101(4) 0.32967(18) 0.2561(3) 0.0206(7) Uani 1 1 d .
C1 C 0.0770(4) 0.5061(2) 0.1521(3) 0.0264(8) Uani 1 1 d .
O3 O 0.3970(3) 0.43466(13) -0.0425(2) 0.0295(6) Uani 1 1 d .
N3 N 0.5845(3) 0.34331(14) 0.2711(3) 0.0197(6) Uani 1 1 d .
O1 O -0.0100(4) 0.55821(17) 0.1240(3) 0.0483(8) Uani 1 1 d .
O2 O -0.0403(3) 0.30566(15) 0.0742(3) 0.0424(7) Uani 1 1 d .
C4 C 0.4074(4) 0.49516(17) 0.2912(3) 0.0169(7) Uani 1 1 d .
N4 N 0.3912(3) 0.25563(15) 0.2968(3) 0.0239(7) Uani 1 1 d .
C3 C 0.3348(4) 0.42957(17) 0.0482(3) 0.0190(7) Uani 1 1 d .
C12 C 0.6651(4) 0.41687(16) 0.2395(3) 0.0207(7) Uani 1 1 d .
H12A H 0.6528 0.4250 0.1530 0.025 Uiso 1 1 calc R
H12B H 0.7910 0.4154 0.2614 0.025 Uiso 1 1 calc R
N2 N 0.3868(3) 0.55904(15) 0.3594(3) 0.0214(6) Uani 1 1 d .
C5 C 0.6670(4) 0.53383(18) 0.3737(3) 0.0239(8) Uani 1 1 d .
H5 H 0.7880 0.5352 0.3940 0.029 Uiso 1 1 calc R
C10 C 0.5484(4) 0.2248(2) 0.3378(4) 0.0319(9) Uani 1 1 d .
H10 H 0.5669 0.1741 0.3709 0.038 Uiso 1 1 calc R
C7 C 0.2221(4) 0.59814(19) 0.3810(4) 0.0297(9) Uani 1 1 d .
H7A H 0.2361 0.6324 0.4502 0.045 Uiso 1 1 calc GR
H7B H 0.1324 0.5587 0.3957 0.045 Uiso 1 1 calc GR
H7C H 0.1869 0.6296 0.3118 0.045 Uiso 1 1 calc GR
C9 C 0.6690(4) 0.27979(18) 0.3222(3) 0.0269(8) Uani 1 1 d .
H9 H 0.7898 0.2759 0.3423 0.032 Uiso 1 1 calc R
C11 C 0.2260(4) 0.2134(2) 0.3001(4) 0.0337(10) Uani 1 1 d .
H11A H 0.1447 0.2426 0.3486 0.051 Uiso 1 1 calc GR
H11B H 0.2459 0.1612 0.3344 0.051 Uiso 1 1 calc GR
H11C H 0.1765 0.2080 0.2196 0.051 Uiso 1 1 calc GR
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'
Cl Cl 0.1484 0.1585 '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'
Re Re -1.0185 7.2310 '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
C2 Re1 Cl1 89.84(11)
C2 Re1 C8 95.91(13)
C2 Re1 C4 175.96(13)
C8 Re1 Cl1 85.81(9)
C8 Re1 C4 82.04(12)
C1 Re1 Cl1 92.90(11)
C1 Re1 C2 90.45(14)
C1 Re1 C8 173.51(13)
C1 Re1 C4 91.54(13)
C4 Re1 Cl1 86.55(8)
C3 Re1 Cl1 177.72(9)
C3 Re1 C2 88.51(14)
C3 Re1 C8 92.81(13)
C3 Re1 C1 88.67(14)
C3 Re1 C4 95.05(12)
O2 C2 Re1 177.2(3)
C4 N1 C12 122.6(3)
C4 N1 C5 112.1(3)
C5 N1 C12 125.3(3)
C5 C6 N2 107.5(3)
N3 C8 Re1 123.1(2)
N4 C8 Re1 133.2(2)
N4 C8 N3 103.4(3)
O1 C1 Re1 178.4(3)
C8 N3 C12 122.9(3)
C8 N3 C9 111.4(3)
C9 N3 C12 125.7(3)
N1 C4 Re1 123.0(2)
N2 C4 Re1 133.4(2)
N2 C4 N1 103.3(3)
C8 N4 C10 111.5(3)
C8 N4 C11 124.9(3)
C10 N4 C11 123.6(3)
O3 C3 Re1 177.9(3)
N3 C12 N1 109.7(2)
C6 N2 C7 123.2(3)
C4 N2 C6 111.0(3)
C4 N2 C7 125.8(3)
C6 C5 N1 106.0(3)
C9 C10 N4 106.9(3)
C10 C9 N3 106.8(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Re1 Cl1 2.5223(8)
Re1 C2 1.948(4)
Re1 C8 2.167(3)
Re1 C1 1.934(4)
Re1 C4 2.173(3)
Re1 C3 1.892(4)
C2 O2 1.148(4)
N1 C4 1.366(4)
N1 C12 1.452(4)
N1 C5 1.370(4)
C6 N2 1.385(4)
C6 C5 1.335(5)
C8 N3 1.364(4)
C8 N4 1.353(4)
C1 O1 1.150(4)
O3 C3 1.150(4)
N3 C12 1.448(4)
N3 C9 1.379(4)
C4 N2 1.347(4)
N4 C10 1.382(4)
N4 C11 1.460(4)
N2 C7 1.457(4)
C10 C9 1.333(4)
