#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:09:38 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179096 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/58/4305818.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_4305818
loop_
_publ_author_name
'Marina K. Kuimova'
'Wassim Z. Alsindi'
'Alexander J. Blake'
'E. Stephen Davies'
'Daniele J. Lampus'
'Pavel Matousek'
'Jonathan McMaster'
'Anthony W. Parker'
'Michael Towrie'
'Xue-Zhong Sun'
'Claire Wilson'
'Michael W. George'
_publ_section_title
;
Probing the Solvent Dependent Photophysics of fac-[Re(CO)3(dppz-X2)Cl]
(dppz-X2= 11,12-X2-dipyrido[3,2-a:2',3'-c]phenazine); X = CH3, H, F,
Cl, CF3)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9857
_journal_page_last               9869
_journal_paper_doi               10.1021/ic800753f
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C21 H8 Cl F2 N4 O3 Re'
_chemical_formula_sum            'C21 H8 Cl F2 N4 O3 Re'
_chemical_formula_weight         623.96
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'enCIFer editing of SHELXL97 CIF output'
_cell_angle_alpha                90.00
_cell_angle_beta                 97.7463(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.4966(2)
_cell_length_b                   23.2065(6)
_cell_length_c                   12.7762(3)
_cell_measurement_reflns_used    4439
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      55.0
_cell_measurement_theta_min      5.8
_cell_volume                     1908.61(9)
_computing_cell_refinement
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, 1998)'
_computing_data_collection       'COLLECT (Hooft, 1998)'
_computing_data_reduction        DENZO
_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      120(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type
'Bruker-Nonius 95mm CCD camera on κ-goniostat'
_diffrn_measurement_method       'φ & ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.046
_diffrn_reflns_av_sigmaI/netI    0.031
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            27640
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         3.22
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.560
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.772
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS V2.10; Sheldrick, 2003)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    2.171
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Blade
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.01
_refine_diff_density_max         2.26
_refine_diff_density_min         -0.86
_refine_diff_density_rms         0.14
_refine_ls_extinction_coef       0.00058(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.17
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         4378
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.17
_refine_ls_R_factor_all          0.0372
_refine_ls_R_factor_gt           0.0312
_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)+(0.004P)²+10.99P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0634
_refine_ls_wR_factor_ref         0.0654
_reflns_number_gt                3975
_reflns_number_total             4378
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800753f_si_002_2.cif
_cod_data_source_block           redpf2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4305818
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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
Re Re 0.33559(3) -0.083386(8) 0.290133(14) 0.01483(7) Uani 1 1 d . . .
Cl Cl 0.09839(19) -0.09401(5) 0.12237(9) 0.0216(2) Uani 1 1 d . . .
C1C C 0.1765(8) -0.1388(2) 0.3576(4) 0.0229(11) Uani 1 1 d . . .
O1C O 0.0795(6) -0.17176(18) 0.3962(3) 0.0395(11) Uani 1 1 d . . .
C2C C 0.5108(8) -0.1458(2) 0.2567(4) 0.0232(11) Uani 1 1 d . . .
O2C O 0.6139(7) -0.18359(18) 0.2384(3) 0.0418(11) Uani 1 1 d . . .
C3C C 0.5154(8) -0.0713(2) 0.4235(4) 0.0229(11) Uani 1 1 d . . .
O3C O 0.6143(6) -0.06591(17) 0.4987(3) 0.0311(9) Uani 1 1 d . . .
N1 N 0.1433(6) -0.00882(16) 0.3099(3) 0.0131(8) Uani 1 1 d . . .
C2 C -0.0149(7) -0.0058(2) 0.3666(3) 0.0159(9) Uani 1 1 d . . .
H2 H -0.0440 -0.0384 0.4071 0.019 Uiso 1 1 calc R . .
C3 C -0.1388(7) 0.0429(2) 0.3692(3) 0.0163(9) Uani 1 1 d . . .
H3 H -0.2451 0.0439 0.4134 0.020 Uiso 1 1 calc R . .
C4 C -0.1064(7) 0.0895(2) 0.3072(3) 0.0169(9) Uani 1 1 d . . .
H4 H -0.1910 0.1229 0.3073 0.020 Uiso 1 1 calc R . .
C5 C 0.0537(7) 0.0869(2) 0.2438(3) 0.0146(9) Uani 1 1 d . . .
C6 C 0.1793(7) 0.0380(2) 0.2498(3) 0.0141(9) Uani 1 1 d . . .
C7 C 0.0855(7) 0.13136(19) 0.1668(3) 0.0148(9) Uani 1 1 d . . .
N8 N -0.0633(6) 0.17120(17) 0.1469(3) 0.0166(8) Uani 1 1 d . . .
C9 C -0.0402(8) 0.2088(2) 0.0690(4) 0.0178(10) Uani 1 1 d . . .
C10 C -0.2066(8) 0.2475(2) 0.0363(4) 0.0231(10) Uani 1 1 d . . .
H10 H -0.3265 0.2484 0.0714 0.028 Uiso 1 1 calc R . .
C11 C -0.1891(8) 0.2831(2) -0.0461(4) 0.0248(11) Uani 1 1 d . . .
F11 F -0.3440(5) 0.31896(15) -0.0838(3) 0.0354(8) Uani 1 1 d . . .
C12 C -0.0084(8) 0.2838(2) -0.0963(4) 0.0238(11) Uani 1 1 d . . .
F12 F -0.0053(5) 0.32188(14) -0.1762(3) 0.0336(8) Uani 1 1 d . . .
C13 C 0.1545(8) 0.2482(2) -0.0673(4) 0.0219(10) Uani 1 1 d . . .
H13 H 0.2757 0.2498 -0.1013 0.026 Uiso 1 1 calc R . .
C14 C 0.1379(7) 0.2083(2) 0.0157(4) 0.0166(9) Uani 1 1 d . . .
N15 N 0.2898(6) 0.16834(17) 0.0380(3) 0.0167(8) Uani 1 1 d . . .
C16 C 0.2591(7) 0.1287(2) 0.1103(3) 0.0145(9) Uani 1 1 d . . .
C17 C 0.4019(7) 0.0796(2) 0.1263(3) 0.0147(9) Uani 1 1 d . . .
C18 C 0.5767(7) 0.0742(2) 0.0731(3) 0.0160(9) Uani 1 1 d . . .
H18 H 0.6133 0.1040 0.0280 0.019 Uiso 1 1 calc R . .
C19 C 0.6939(7) 0.0245(2) 0.0878(3) 0.0159(9) Uani 1 1 d . . .
H19 H 0.8146 0.0203 0.0540 0.019 Uiso 1 1 calc R . .
C20 C 0.6355(7) -0.0196(2) 0.1525(3) 0.0148(9) Uani 1 1 d . . .
H20 H 0.7168 -0.0537 0.1608 0.018 Uiso 1 1 calc R . .
N21 N 0.4682(6) -0.01515(16) 0.2029(3) 0.0129(7) Uani 1 1 d . . .
C22 C 0.3565(7) 0.03420(19) 0.1914(3) 0.0136(9) 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'
F F 0.0171 0.0103 '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'
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
_geom_angle_publ_flag
C1C Re C2C 88.0(2) . . ?
C1C Re C3C 89.9(2) . . ?
C2C Re C3C 90.0(2) . . ?
C1C Re N1 97.36(18) . . ?
C2C Re N1 173.29(17) . . ?
C3C Re N1 94.02(17) . . ?
C1C Re N21 170.90(18) . . ?
C2C Re N21 98.47(18) . . ?
C3C Re N21 96.39(17) . . ?
N1 Re N21 75.73(14) . . ?
C1C Re Cl 90.70(15) . . ?
C2C Re Cl 92.92(15) . . ?
C3C Re Cl 177.08(15) . . ?
N1 Re Cl 83.08(10) . . ?
N21 Re Cl 82.67(10) . . ?
O1C C1C Re 178.8(5) . . ?
O2C C2C Re 178.7(5) . . ?
O3C C3C Re 178.3(5) . . ?
C2 N1 C6 117.7(4) . . ?
C2 N1 Re 127.1(3) . . ?
C6 N1 Re 115.0(3) . . ?
N1 C2 C3 123.1(4) . . ?
N1 C2 H2 118.4 . . ?
C3 C2 H2 118.4 . . ?
C4 C3 C2 119.5(4) . . ?
C4 C3 H3 120.2 . . ?
C2 C3 H3 120.2 . . ?
C3 C4 C5 118.8(4) . . ?
C3 C4 H4 120.6 . . ?
C5 C4 H4 120.6 . . ?
C6 C5 C4 118.5(4) . . ?
C6 C5 C7 118.5(4) . . ?
C4 C5 C7 122.9(4) . . ?
N1 C6 C5 122.3(4) . . ?
N1 C6 C22 116.6(4) . . ?
C5 C6 C22 121.2(4) . . ?
N8 C7 C16 122.5(4) . . ?
N8 C7 C5 116.9(4) . . ?
C16 C7 C5 120.4(4) . . ?
C7 N8 C9 116.0(4) . . ?
N8 C9 C14 121.9(4) . . ?
N8 C9 C10 118.0(4) . . ?
C14 C9 C10 120.0(4) . . ?
C11 C10 C9 118.2(5) . . ?
C11 C10 H10 120.9 . . ?
C9 C10 H10 120.9 . . ?
F11 C11 C10 121.2(5) . . ?
F11 C11 C12 117.3(4) . . ?
C10 C11 C12 121.5(5) . . ?
F12 C12 C13 120.9(5) . . ?
F12 C12 C11 116.6(4) . . ?
C13 C12 C11 122.4(5) . . ?
C12 C13 C14 117.7(5) . . ?
C12 C13 H13 121.1 . . ?
C14 C13 H13 121.1 . . ?
N15 C14 C9 121.5(4) . . ?
N15 C14 C13 118.4(4) . . ?
C9 C14 C13 120.1(4) . . ?
C16 N15 C14 116.3(4) . . ?
N15 C16 C7 121.5(4) . . ?
N15 C16 C17 118.7(4) . . ?
C7 C16 C17 119.7(4) . . ?
C22 C17 C18 117.9(4) . . ?
C22 C17 C16 119.2(4) . . ?
C18 C17 C16 122.7(4) . . ?
C19 C18 C17 118.5(4) . . ?
C19 C18 H18 120.8 . . ?
C17 C18 H18 120.8 . . ?
C18 C19 C20 120.2(4) . . ?
C18 C19 H19 119.9 . . ?
C20 C19 H19 119.9 . . ?
N21 C20 C19 121.9(4) . . ?
N21 C20 H20 119.0 . . ?
C19 C20 H20 119.0 . . ?
C20 N21 C22 118.1(4) . . ?
C20 N21 Re 126.3(3) . . ?
C22 N21 Re 115.3(3) . . ?
N21 C22 C17 123.3(4) . . ?
N21 C22 C6 116.4(4) . . ?
C17 C22 C6 120.3(4) . . ?
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
Re C1C 1.925(5) . ?
Re C2C 1.926(5) . ?
Re C3C 1.952(6) . ?
Re N1 2.169(4) . ?
Re N21 2.180(4) . ?
Re Cl 2.4777(12) . ?
C1C O1C 1.144(6) . ?
C2C O2C 1.146(6) . ?
C3C O3C 1.089(6) . ?
N1 C2 1.337(6) . ?
N1 C6 1.368(6) . ?
C2 C3 1.389(7) . ?
C2 H2 0.9500 . ?
C3 C4 1.373(7) . ?
C3 H3 0.9500 . ?
C4 C5 1.403(6) . ?
C4 H4 0.9500 . ?
C5 C6 1.396(6) . ?
C5 C7 1.459(6) . ?
C6 C22 1.456(6) . ?
C7 N8 1.337(6) . ?
C7 C16 1.420(6) . ?
N8 C9 1.347(6) . ?
C9 C14 1.419(7) . ?
C9 C10 1.424(7) . ?
C10 C11 1.355(7) . ?
C10 H10 0.9500 . ?
C11 F11 1.344(6) . ?
C11 C12 1.411(7) . ?
C12 F12 1.353(6) . ?
C12 C13 1.354(7) . ?
C13 C14 1.423(7) . ?
C13 H13 0.9500 . ?
C14 N15 1.356(6) . ?
N15 C16 1.338(6) . ?
C16 C17 1.465(6) . ?
C17 C22 1.399(6) . ?
C17 C18 1.405(6) . ?
C18 C19 1.380(7) . ?
C18 H18 0.9500 . ?
C19 C20 1.400(6) . ?
C19 H19 0.9500 . ?
C20 N21 1.340(6) . ?
C20 H20 0.9500 . ?
N21 C22 1.353(6) . ?
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
C6 N1 C2 C3 -1.8(6) . . . . ?
N1 C2 C3 C4 3.2(7) . . . . ?
C2 C3 C4 C5 -0.8(7) . . . . ?
C3 C4 C5 C6 -2.7(6) . . . . ?
C3 C4 C5 C7 173.0(4) . . . . ?
C2 N1 C6 C5 -2.0(6) . . . . ?
C2 N1 C6 C22 178.1(4) . . . . ?
C4 C5 C6 N1 4.2(7) . . . . ?
C7 C5 C6 N1 -171.6(4) . . . . ?
C4 C5 C6 C22 -175.9(4) . . . . ?
C7 C5 C6 C22 8.3(6) . . . . ?
C6 C5 C7 N8 165.9(4) . . . . ?
C4 C5 C7 N8 -9.7(6) . . . . ?
C6 C5 C7 C16 -9.0(6) . . . . ?
C4 C5 C7 C16 175.4(4) . . . . ?
C16 C7 N8 C9 0.5(6) . . . . ?
C5 C7 N8 C9 -174.3(4) . . . . ?
C7 N8 C9 C14 -3.8(7) . . . . ?
C7 N8 C9 C10 172.6(4) . . . . ?
N8 C9 C10 C11 -176.2(5) . . . . ?
C14 C9 C10 C11 0.2(7) . . . . ?
C9 C10 C11 F11 177.1(5) . . . . ?
C9 C10 C11 C12 -2.5(8) . . . . ?
F11 C11 C12 F12 1.8(7) . . . . ?
C10 C11 C12 F12 -178.5(5) . . . . ?
F11 C11 C12 C13 -177.8(5) . . . . ?
C10 C11 C12 C13 1.9(9) . . . . ?
F12 C12 C13 C14 -178.5(4) . . . . ?
C11 C12 C13 C14 1.1(8) . . . . ?
N8 C9 C14 N15 2.7(7) . . . . ?
C10 C9 C14 N15 -173.6(4) . . . . ?
N8 C9 C14 C13 179.0(4) . . . . ?
C10 C9 C14 C13 2.7(7) . . . . ?
C12 C13 C14 N15 173.1(5) . . . . ?
C12 C13 C14 C9 -3.3(7) . . . . ?
C9 C14 N15 C16 1.9(6) . . . . ?
C13 C14 N15 C16 -174.4(4) . . . . ?
C14 N15 C16 C7 -5.2(6) . . . . ?
C14 N15 C16 C17 171.1(4) . . . . ?
N8 C7 C16 N15 4.3(7) . . . . ?
C5 C7 C16 N15 178.9(4) . . . . ?
N8 C7 C16 C17 -172.0(4) . . . . ?
C5 C7 C16 C17 2.6(6) . . . . ?
N15 C16 C17 C22 -171.9(4) . . . . ?
C7 C16 C17 C22 4.5(6) . . . . ?
N15 C16 C17 C18 3.7(7) . . . . ?
C7 C16 C17 C18 -180.0(4) . . . . ?
C22 C17 C18 C19 0.0(6) . . . . ?
C16 C17 C18 C19 -175.6(4) . . . . ?
C17 C18 C19 C20 1.5(7) . . . . ?
C18 C19 C20 N21 -1.0(7) . . . . ?
C19 C20 N21 C22 -1.1(6) . . . . ?
C19 C20 N21 Re 172.0(3) . . . . ?
C1C Re N21 C20 -140.8(11) . . . . ?
C2C Re N21 C20 -5.5(4) . . . . ?
C3C Re N21 C20 85.4(4) . . . . ?
N1 Re N21 C20 178.0(4) . . . . ?
Cl Re N21 C20 -97.3(4) . . . . ?
C1C Re N21 C22 32.5(13) . . . . ?
C2C Re N21 C22 167.9(3) . . . . ?
C3C Re N21 C22 -101.2(3) . . . . ?
N1 Re N21 C22 -8.7(3) . . . . ?
Cl Re N21 C22 76.0(3) . . . . ?
C20 N21 C22 C17 2.8(6) . . . . ?
Re N21 C22 C17 -171.2(3) . . . . ?
C20 N21 C22 C6 -178.4(4) . . . . ?
C18 C17 C22 N21 -2.2(7) . . . . ?
C16 C17 C22 N21 173.5(4) . . . . ?
C18 C17 C22 C6 179.0(4) . . . . ?
C16 C17 C22 C6 -5.3(6) . . . . ?
N1 C6 C22 N21 -0.2(6) . . . . ?
C5 C6 C22 N21 179.9(4) . . . . ?
N1 C6 C22 C17 178.7(4) . . . . ?
C5 C6 C22 C17 -1.2(7) . . . . ?
