#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/58/4305817.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_4305817
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 Cl3 N4 O3 Re, 0.5(C4 H8 O)'
_chemical_formula_sum            'C23 H12 Cl3 N4 O3.5 Re'
_chemical_formula_weight         692.92
_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           'enCIFer editing of SHELXL97 CIF output'
_cell_angle_alpha                90.00
_cell_angle_beta                 116.562(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.958(2)
_cell_length_b                   18.054(2)
_cell_length_c                   13.530(2)
_cell_measurement_reflns_used    7240
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.25
_cell_volume                     4360.6(9)
_computing_cell_refinement       'Bruker SAINT version 6.02a (Bruker, 2000)'
_computing_data_collection       'Bruker SMART version 5.624 (Bruker, 2001)'
_computing_data_reduction        'Bruker SAINT; Bruker SHELXTL (Bruker, 2001)'
_computing_publication_material
'enCIFer (Allen et al., 2004; PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Bruker SMART1000 CCD area detector'
_diffrn_measurement_method       omega
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.024
_diffrn_reflns_av_sigmaI/netI    0.030
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13248
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.92
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.981
_exptl_absorpt_correction_T_max  0.740
_exptl_absorpt_correction_T_min  0.454
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Sadabs v2.03; Bruker, 2002)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.111
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       column
_exptl_crystal_F_000             2656
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.09
_refine_diff_density_min         -1.57
_refine_diff_density_rms         0.13
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         4906
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0350
_refine_ls_R_factor_gt           0.0261
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0376P)²+14.15P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0658
_refine_ls_wR_factor_ref         0.0722
_reflns_number_gt                4176
_reflns_number_total             4906
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ic800753f_si_002_1.cif
_cod_data_source_block           (3)
_cod_original_cell_volume        4360.6(15)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C23 H12 Cl3 N4 O3.50 Re'
_cod_database_code               4305817
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
Re1 Re -0.341515(8) 0.658919(8) 0.580741(12) 0.02144(6) Uani 1 1 d . . .
Cl1 Cl 0.25293(6) 0.39994(6) 1.06478(9) 0.0313(2) Uani 1 1 d . . .
Cl2 Cl 0.16113(6) 0.25243(6) 1.01848(10) 0.0346(2) Uani 1 1 d . . .
Cl3 Cl -0.30748(7) 0.60651(5) 0.44010(8) 0.0336(2) Uani 1 1 d . . .
C1C C -0.3622(2) 0.7575(2) 0.5204(3) 0.0241(8) Uani 1 1 d . . .
O1C O -0.37438(18) 0.81703(17) 0.4872(3) 0.0315(7) Uani 1 1 d . . .
C2C C -0.4454(3) 0.6384(3) 0.4948(5) 0.0478(14) Uani 1 1 d . . .
O2C O -0.5086(2) 0.6282(3) 0.4427(5) 0.093(2) Uani 1 1 d . . .
O3C O -0.3790(3) 0.7197(3) 0.7603(4) 0.0836(18) Uani 1 1 d . . .
C3C C -0.3636(3) 0.6955(3) 0.6961(4) 0.0441(13) Uani 1 1 d . . .
C1 C -0.2358(2) 0.4105(2) 0.7250(3) 0.0253(8) Uani 1 1 d . . .
H1A H -0.2138 0.3631 0.7485 0.030 Uiso 1 1 calc R . .
C2 C -0.3125(2) 0.4185(2) 0.6721(4) 0.0299(9) Uani 1 1 d . . .
H2A H -0.3440 0.3767 0.6602 0.036 Uiso 1 1 calc R . .
C3 C -0.3435(2) 0.4883(2) 0.6362(4) 0.0275(9) Uani 1 1 d . . .
H3A H -0.3965 0.4930 0.5994 0.033 Uiso 1 1 calc R . .
N4 N -0.30155(18) 0.54912(17) 0.6516(3) 0.0205(6) Uani 1 1 d . . .
C4A C -0.2257(2) 0.5414(2) 0.7054(3) 0.0192(7) Uani 1 1 d . . .
C4B C -0.1824(2) 0.60899(19) 0.7221(3) 0.0167(7) Uani 1 1 d . . .
N5 N -0.22153(19) 0.67190(17) 0.6787(3) 0.0182(6) Uani 1 1 d . . .
C6 C -0.1834(2) 0.7356(2) 0.6945(3) 0.0225(8) Uani 1 1 d . . .
H6A H -0.2103 0.7797 0.6628 0.027 Uiso 1 1 calc R . .
C7 C -0.1062(2) 0.7393(2) 0.7556(3) 0.0235(8) Uani 1 1 d . . .
H7A H -0.0812 0.7856 0.7669 0.028 Uiso 1 1 calc R . .
C8B C -0.0666(2) 0.5377(2) 0.8213(3) 0.0171(7) Uani 1 1 d . . .
C8 C -0.0658(2) 0.6756(2) 0.7997(3) 0.0208(8) Uani 1 1 d . . .
H8A H -0.0129 0.6773 0.8412 0.025 Uiso 1 1 calc R . .
C8A C -0.1045(2) 0.6081(2) 0.7821(3) 0.0174(7) Uani 1 1 d . . .
N9 N 0.00774(18) 0.53832(17) 0.8751(2) 0.0192(6) Uani 1 1 d . . .
C9A C 0.0419(2) 0.4716(2) 0.9068(3) 0.0191(7) Uani 1 1 d . . .
C10 C 0.1216(2) 0.4694(2) 0.9644(3) 0.0219(8) Uani 1 1 d . . .
H10A H 0.1499 0.5140 0.9802 0.026 Uiso 1 1 calc R . .
C11 C 0.1569(2) 0.4028(2) 0.9963(3) 0.0228(8) Uani 1 1 d . . .
C12 C 0.1149(2) 0.3355(2) 0.9737(3) 0.0228(8) Uani 1 1 d . . .
C13 C 0.0383(2) 0.3364(2) 0.9184(3) 0.0240(8) Uani 1 1 d . . .
H13A H 0.0110 0.2913 0.9029 0.029 Uiso 1 1 calc R . .
C13A C 0.0002(2) 0.4044(2) 0.8843(3) 0.0194(7) Uani 1 1 d . . .
N14 N -0.07562(18) 0.40472(17) 0.8310(3) 0.0207(7) Uani 1 1 d . . .
C14B C -0.1907(2) 0.4737(2) 0.7437(3) 0.0192(7) Uani 1 1 d . . .
C14A C -0.1087(2) 0.4705(2) 0.8003(3) 0.0182(7) Uani 1 1 d . . .
O1S O -0.4979(5) 0.4807(4) 0.3751(6) 0.054(2) Uani 0.50 1 d PD A -1
C2S C -0.5204(7) 0.5216(6) 0.2742(8) 0.054(3) Uani 0.50 1 d PD A -1
H2SA H -0.4794 0.5543 0.2787 0.065 Uiso 0.50 1 calc PR A -1
H2SB H -0.5649 0.5524 0.2597 0.065 Uiso 0.50 1 calc PR A -1
C3S C -0.5394(7) 0.4632(6) 0.1806(11) 0.073(5) Uani 0.50 1 d PD A -1
H3SA H -0.5898 0.4413 0.1565 0.087 Uiso 0.50 1 calc PR A -1
H3SB H -0.5347 0.4836 0.1161 0.087 Uiso 0.50 1 calc PR A -1
C4S C -0.4765(7) 0.4083(7) 0.2470(9) 0.062(3) Uani 0.50 1 d PD A -1
H4SA H -0.4331 0.4161 0.2312 0.075 Uiso 0.50 1 calc PR A -1
H4SB H -0.4943 0.3567 0.2271 0.075 Uiso 0.50 1 calc PR A -1
C5S C -0.4538(5) 0.4228(5) 0.3706(7) 0.037(2) Uani 0.50 1 d PD A -1
H5SB H -0.4624 0.3779 0.4055 0.044 Uiso 0.50 1 calc PR A -1
H5SA H -0.4001 0.4362 0.4101 0.044 Uiso 0.50 1 calc PR A -1
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'
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
C2C Re1 C3C 88.9(3) . . ?
C2C Re1 C1C 87.29(19) . . ?
C3C Re1 C1C 86.76(19) . . ?
C2C Re1 N5 174.96(18) . . ?
C3C Re1 N5 93.33(19) . . ?
C1C Re1 N5 97.34(15) . . ?
C2C Re1 N4 100.07(17) . . ?
C3C Re1 N4 97.29(17) . . ?
C1C Re1 N4 171.63(15) . . ?
N5 Re1 N4 75.17(12) . . ?
C2C Re1 Cl3 93.1(2) . . ?
C3C Re1 Cl3 176.53(14) . . ?
C1C Re1 Cl3 96.17(12) . . ?
N5 Re1 Cl3 84.46(9) . . ?
N4 Re1 Cl3 79.57(9) . . ?
O1C C1C Re1 178.0(4) . . ?
O2C C2C Re1 178.0(5) . . ?
O3C C3C Re1 176.4(4) . . ?
C2 C1 C14B 118.8(4) . . ?
C1 C2 C3 119.7(4) . . ?
N4 C3 C2 122.5(4) . . ?
C3 N4 C4A 117.9(3) . . ?
C3 N4 Re1 126.4(3) . . ?
C4A N4 Re1 115.2(2) . . ?
N4 C4A C14B 122.9(3) . . ?
N4 C4A C4B 116.0(3) . . ?
C14B C4A C4B 121.1(3) . . ?
N5 C4B C8A 122.6(3) . . ?
N5 C4B C4A 116.7(3) . . ?
C8A C4B C4A 120.7(3) . . ?
C6 N5 C4B 118.2(3) . . ?
C6 N5 Re1 125.6(3) . . ?
C4B N5 Re1 116.0(2) . . ?
N5 C6 C7 122.5(4) . . ?
C8 C7 C6 119.7(4) . . ?
N9 C8B C14A 122.0(3) . . ?
N9 C8B C8A 117.6(3) . . ?
C14A C8B C8A 120.4(3) . . ?
C7 C8 C8A 118.7(4) . . ?
C4B C8A C8 118.2(3) . . ?
C4B C8A C8B 119.0(3) . . ?
C8 C8A C8B 122.7(3) . . ?
C8B N9 C9A 116.5(3) . . ?
N9 C9A C13A 121.7(3) . . ?
N9 C9A C10 118.5(3) . . ?
C13A C9A C10 119.7(3) . . ?
C11 C10 C9A 119.3(4) . . ?
C10 C11 C12 120.8(4) . . ?
C10 C11 Cl1 119.4(3) . . ?
C12 C11 Cl1 119.7(3) . . ?
C13 C12 C11 120.8(4) . . ?
C13 C12 Cl2 119.6(3) . . ?
C11 C12 Cl2 119.6(3) . . ?
C12 C13 C13A 119.8(4) . . ?
N14 C13A C13 119.3(3) . . ?
N14 C13A C9A 121.1(3) . . ?
C13 C13A C9A 119.6(4) . . ?
C14A N14 C13A 116.8(3) . . ?
C4A C14B C1 118.3(4) . . ?
C4A C14B C14A 119.2(3) . . ?
C1 C14B C14A 122.5(3) . . ?
N14 C14A C8B 121.9(3) . . ?
N14 C14A C14B 118.8(3) . . ?
C8B C14A C14B 119.3(3) . . ?
C5S O1S C2S 106.3(8) . . ?
O1S C2S C3S 106.5(8) . . ?
C4S C3S C2S 97.1(9) . . ?
C3S C4S C5S 106.9(9) . . ?
O1S C5S C4S 106.9(7) . . ?
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
Re1 C1C 1.924(4) . ?
Re1 C2C 1.906(5) . ?
Re1 C3C 1.919(5) . ?
Re1 N4 2.191(3) . ?
Re1 N5 2.170(3) . ?
Re1 Cl3 2.4766(11) . ?
Cl1 C11 1.717(4) . ?
Cl2 C12 1.723(4) . ?
C1C O1C 1.148(5) . ?
C2C O2C 1.151(6) . ?
O3C C3C 1.131(6) . ?
C1 C2 1.377(6) . ?
C1 C14B 1.405(5) . ?
C2 C3 1.393(6) . ?
C3 N4 1.340(5) . ?
N4 C4A 1.362(5) . ?
C4A C14B 1.388(5) . ?
C4A C4B 1.453(5) . ?
C4B N5 1.354(5) . ?
C4B C8A 1.395(5) . ?
N5 C6 1.342(5) . ?
C6 C7 1.387(6) . ?
C7 C8 1.377(5) . ?
C8B N9 1.329(5) . ?
C8B C14A 1.430(5) . ?
C8B C8A 1.453(5) . ?
C8 C8A 1.405(5) . ?
N9 C9A 1.355(5) . ?
C9A C13A 1.426(5) . ?
C9A C10 1.426(5) . ?
C10 C11 1.363(6) . ?
C11 C12 1.429(6) . ?
C12 C13 1.369(6) . ?
C13 C13A 1.408(5) . ?
C13A N14 1.354(5) . ?
N14 C14A 1.332(5) . ?
C14B C14A 1.465(5) . ?
O1S C5S 1.386(7) . ?
O1S C2S 1.436(7) . ?
C2S C3S 1.558(14) . ?
C3S C4S 1.535(12) . ?
C4S C5S 1.548(12) . ?
