#------------------------------------------------------------------------------
#$Date: 2015-12-09 16:29:51 +0200 (Wed, 09 Dec 2015) $
#$Revision: 171207 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/67/7036793.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_7036793
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         'C18 H16 Cl N4 O3 Re, C H Cl3'
_chemical_formula_sum            'C19 H17 Cl4 N4 O3 Re'
_chemical_formula_weight         677.36
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_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
_audit_creation_date             2015-07-07
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.0212(4)
_cell_length_b                   12.3025(4)
_cell_length_c                   12.4828(3)
_cell_measurement_temperature    173
_cell_volume                     2306.80(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      173
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0301
_diffrn_reflns_av_unetI/netI     0.0156
_diffrn_reflns_laue_measured_fraction_full 0.998
_diffrn_reflns_laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            19918
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         3.165
_exptl_absorpt_coefficient_mu    5.760
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89016
_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 light green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.950
_exptl_crystal_description       plate
_exptl_crystal_F_000             1304
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.129
_refine_diff_density_min         -2.180
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         2472
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0268
_refine_ls_R_factor_gt           0.0236
_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)+(0.0251P)²+9.2713P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0555
_refine_ls_wR_factor_ref         0.0580
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2281
_reflns_number_total             2472
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5dt03295d2.cif
_cod_data_source_block           trans-15
_cod_depositor_comments
'Adding full bibliography for 7036787--7036794.cif.'
_cod_original_cell_volume        2306.80(10)
_cod_database_code               7036793
_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
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C4(H4), C12(H12)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C2(H2), C3(H3), C8(H8)
2.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C)
;
_olex2_date_sample_data_collection 2014-07-29
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, z'
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
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Re1 Re 0.83194(2) 0.2500 0.46816(2) 0.01685(7) Uani 1 2 d S T P
Cl1 Cl 0.92803(9) 0.2500 0.30243(11) 0.0313(3) Uani 1 2 d S T P
O2 O 0.7260(3) 0.2500 0.6764(3) 0.0269(8) Uani 1 2 d S T P
N1 N 0.66656(18) 0.3466(2) 0.3433(2) 0.0192(6) Uani 1 1 d . . .
C5 C 0.5776(3) 0.2500 0.4804(4) 0.0244(11) Uani 1 2 d S T P
C10 C 0.9060(2) 0.3586(3) 0.5369(3) 0.0255(8) Uani 1 1 d . . .
N2 N 0.7694(2) 0.4649(3) 0.3403(3) 0.0269(7) Uani 1 1 d . . .
O1 O 0.9495(2) 0.4193(3) 0.5836(2) 0.0414(8) Uani 1 1 d . . .
C4 C 0.6145(3) 0.2500 0.3669(4) 0.0188(10) Uani 1 2 d S T P
H4 H 0.5625 0.2500 0.3170 0.023 Uiso 1 2 calc RS T P
C6 C 0.5576(3) 0.3472(4) 0.5307(3) 0.0349(10) Uani 1 1 d . . .
H6 H 0.5705 0.4143 0.4963 0.042 Uiso 1 1 calc R . .
C7 C 0.5187(3) 0.3463(5) 0.6318(4) 0.0528(14) Uani 1 1 d . . .
H7 H 0.5053 0.4130 0.6665 0.063 Uiso 1 1 calc R . .
C1 C 0.7506(2) 0.3655(3) 0.3806(3) 0.0203(7) Uani 1 1 d . . .
C2 C 0.6350(3) 0.4312(3) 0.2820(3) 0.0279(8) Uani 1 1 d . . .
H2 H 0.5789 0.4357 0.2473 0.034 Uiso 1 1 calc R . .
C11 C 0.7624(3) 0.2500 0.5943(4) 0.0189(10) Uani 1 2 d S T P
C3 C 0.6996(3) 0.5057(4) 0.2813(4) 0.0355(10) Uani 1 1 d . . .
H3 H 0.6978 0.5744 0.2465 0.043 Uiso 1 1 calc R . .
C9 C 0.8532(3) 0.5233(4) 0.3550(4) 0.0377(10) Uani 1 1 d . . .
H9A H 0.8578 0.5482 0.4294 0.057 Uiso 1 1 calc GR . .
H9B H 0.8548 0.5862 0.3069 0.057 Uiso 1 1 calc GR . .
H9C H 0.9031 0.4749 0.3387 0.057 Uiso 1 1 calc GR . .
C8 C 0.4994(5) 0.2500 0.6817(5) 0.058(2) Uani 1 2 d S T P
H8 H 0.4727 0.2500 0.7507 0.070 Uiso 1 2 calc RS T P
C12 C 0.7716(5) 0.2500 0.0938(6) 0.060(2) Uani 1 2 d S T P
H12 H 0.7826 0.2500 0.1728 0.072 Uiso 1 2 calc RS T P
Cl2 Cl 0.65564(11) 0.2500 0.07477(14) 0.0499(4) Uani 1 2 d S T P
Cl3 Cl 0.81826(14) 0.3679(3) 0.0427(2) 0.1782(19) 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'
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
C10 Re1 Cl1 91.99(11) 8_565 .
C10 Re1 Cl1 91.99(11) . .
C10 Re1 C10 87.1(2) . 8_565
C10 Re1 C1 95.44(15) . .
C10 Re1 C1 175.93(14) 8_565 .
C10 Re1 C1 95.44(15) 8_565 8_565
C10 Re1 C1 175.93(14) . 8_565
C1 Re1 Cl1 84.78(9) 8_565 .
C1 Re1 Cl1 84.78(9) . .
C1 Re1 C1 81.83(18) 8_565 .
C11 Re1 Cl1 178.67(14) . .
C11 Re1 C10 87.04(15) . 8_565
C11 Re1 C10 87.04(15) . .
C11 Re1 C1 96.22(14) . 8_565
C11 Re1 C1 96.22(14) . .
C1 N1 C4 124.6(3) . .
C1 N1 C2 112.3(3) . .
C2 N1 C4 123.1(3) . .
C6 C5 C4 120.1(3) . .
C6 C5 C4 120.1(3) 8_565 .
C6 C5 C6 119.7(5) 8_565 .
O1 C10 Re1 175.7(3) . .
C1 N2 C3 111.7(3) . .
C1 N2 C9 125.4(3) . .
C3 N2 C9 123.0(3) . .
N1 C4 N1 109.8(4) 8_565 .
N1 C4 C5 112.6(3) 8_565 .
N1 C4 C5 112.6(3) . .
C5 C6 C7 119.7(5) . .
C8 C7 C6 120.6(5) . .
N1 C1 Re1 125.5(3) . .
N2 C1 Re1 131.4(3) . .
N2 C1 N1 102.7(3) . .
C3 C2 N1 105.8(3) . .
O2 C11 Re1 174.5(4) . .
C2 C3 N2 107.4(4) . .
C7 C8 C7 119.7(6) 8_565 .
Cl3 C12 Cl2 110.6(3) 8_565 .
Cl3 C12 Cl2 110.6(3) . .
Cl3 C12 Cl3 113.7(5) 8_565 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Re1 Cl1 2.5225(13) .
Re1 C10 1.939(4) .
Re1 C10 1.939(4) 8_565
Re1 C1 2.169(4) 8_565
Re1 C1 2.169(4) .
Re1 C11 1.889(5) .
O2 C11 1.161(6) .
N1 C4 1.453(4) .
N1 C1 1.365(4) .
N1 C2 1.376(5) .
C5 C4 1.522(7) .
C5 C6 1.383(5) .
C5 C6 1.383(5) 8_565
C10 O1 1.151(5) .
N2 C1 1.352(5) .
N2 C3 1.377(5) .
N2 C9 1.460(5) .
C4 N1 1.453(4) 8_565
C6 C7 1.391(6) .
C7 C8 1.370(7) .
C2 C3 1.335(6) .
C8 C7 1.370(7) 8_565
C12 Cl2 1.758(7) .
C12 Cl3 1.733(5) .
C12 Cl3 1.733(5) 8_565
