#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/58/4305819.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_4305819
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         'C23 H14 Cl N4 O3 Re, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C23.5 H15 Cl2 N4 O3 Re'
_chemical_formula_weight         658.49
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   'geometrically placed, DCM H omitted'
_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                 104.632(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   13.5854(10)
_cell_length_b                   18.1464(13)
_cell_length_c                   18.5411(13)
_cell_measurement_reflns_used    5625
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.55
_cell_measurement_theta_min      2.8
_cell_volume                     4422.6(6)
_computing_cell_refinement       'Bruker SAINT version 6.36a (Bruker, 2000)'
_computing_data_collection       'Bruker SMART version 5.625 (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  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker SMART APEX 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  0.048
_diffrn_reflns_av_sigmaI/netI    0.020
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            18096
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.59
_diffrn_reflns_theta_min         2.24
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.772
_exptl_absorpt_correction_T_max  0.472
_exptl_absorpt_correction_T_min  0.223
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Bruker SHELXTL v6.12)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.978
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2536
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.73
_refine_diff_density_min         -1.19
_refine_diff_density_rms         0.13
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.925
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     308
_refine_ls_number_reflns         5063
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.927
_refine_ls_R_factor_all          0.0303
_refine_ls_R_factor_gt           0.0265
_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)+(0.057P)²+11.241P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0741
_refine_ls_wR_factor_ref         0.0760
_reflns_number_gt                4526
_reflns_number_total             5063
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ic800753f_si_002_3.cif
_cod_data_source_block           (1)
_cod_original_cell_volume        4422.6(9)
_cod_original_sg_symbol_H-M      'I 2/a'
_cod_original_formula_sum        'C23.50 H15 Cl2 N4 O3 Re'
_cod_database_code               4305819
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Re1 Re 0.577754(10) 0.156952(7) 0.155509(7) 0.02124(6) Uani 1 1 d . . .
Cl1 Cl 0.75237(8) 0.10588(6) 0.18956(6) 0.0365(2) Uani 1 1 d . . .
C1C C 0.5650(3) 0.1354(2) 0.0523(2) 0.0313(8) Uani 1 1 d . . .
O1C O 0.5596(3) 0.12436(19) -0.00970(16) 0.0491(9) Uani 1 1 d . . .
C2C C 0.6157(3) 0.2560(2) 0.1358(2) 0.0257(7) Uani 1 1 d . . .
O2C O 0.6365(2) 0.31531(16) 0.12491(16) 0.0355(6) Uani 1 1 d . . .
C3C C 0.4333(4) 0.1921(2) 0.1338(2) 0.0411(12) Uani 1 1 d . . .
O3C O 0.3602(3) 0.2106(2) 0.1157(2) 0.0583(10) Uani 1 1 d . . .
C1 C 0.5349(3) -0.0878(2) 0.2642(2) 0.0264(7) Uani 1 1 d . . .
H1A H 0.5322 -0.1345 0.2868 0.032 Uiso 1 1 calc R . .
C2 C 0.5111(3) -0.0811(2) 0.1877(2) 0.0293(8) Uani 1 1 d . . .
H2A H 0.4905 -0.1230 0.1570 0.035 Uiso 1 1 calc R . .
C3 C 0.5173(3) -0.0122(2) 0.15574(19) 0.0247(7) Uani 1 1 d . . .
H3A H 0.5006 -0.0083 0.1029 0.030 Uiso 1 1 calc R . .
N4 N 0.5459(2) 0.04867(16) 0.19651(15) 0.0205(6) Uani 1 1 d . . .
C4A C 0.5678(3) 0.04183(19) 0.27204(18) 0.0199(7) Uani 1 1 d . . .
C4B C 0.5955(2) 0.10942(19) 0.31490(19) 0.0191(6) Uani 1 1 d . . .
N5 N 0.5996(2) 0.17158(16) 0.27521(17) 0.0205(6) Uani 1 1 d . . .
C6 C 0.6227(3) 0.2354(2) 0.3127(2) 0.0244(7) Uani 1 1 d . . .
H6A H 0.6281 0.2790 0.2856 0.029 Uiso 1 1 calc R . .
C7 C 0.6391(3) 0.2396(2) 0.3899(2) 0.0255(7) Uani 1 1 d . . .
H7A H 0.6531 0.2857 0.4146 0.031 Uiso 1 1 calc R . .
C8B C 0.6115(3) 0.03953(19) 0.43119(18) 0.0204(7) Uani 1 1 d . . .
C8A C 0.6134(2) 0.10920(19) 0.39241(18) 0.0197(7) Uani 1 1 d . . .
C8 C 0.6347(3) 0.1766(2) 0.43011(19) 0.0227(7) Uani 1 1 d . . .
H8A H 0.6459 0.1787 0.4828 0.027 Uiso 1 1 calc R . .
N9 N 0.6326(2) 0.04078(16) 0.50529(16) 0.0217(6) Uani 1 1 d . . .
C9A C 0.6341(3) -0.02461(19) 0.53988(19) 0.0213(7) Uani 1 1 d . . .
C10 C 0.6585(3) -0.0277(2) 0.61876(19) 0.0233(7) Uani 1 1 d . . .
H10A H 0.6722 0.0168 0.6466 0.028 Uiso 1 1 calc R . .
C11 C 0.6627(3) -0.0931(2) 0.65553(19) 0.0245(7) Uani 1 1 d . . .
C11A C 0.6906(3) -0.0951(2) 0.7400(2) 0.0318(8) Uani 1 1 d . . .
H11A H 0.7021 -0.0448 0.7594 0.048 Uiso 1 1 calc R . .
H11B H 0.7528 -0.1242 0.7580 0.048 Uiso 1 1 calc R . .
H11C H 0.6350 -0.1176 0.7572 0.048 Uiso 1 1 calc R . .
C12A C 0.6460(3) -0.2336(2) 0.6541(2) 0.0332(9) Uani 1 1 d . . .
H12A H 0.6239 -0.2730 0.6175 0.050 Uiso 1 1 calc R . .
H12B H 0.6009 -0.2319 0.6878 0.050 Uiso 1 1 calc R . .
H12C H 0.7159 -0.2432 0.6830 0.050 Uiso 1 1 calc R . .
C12 C 0.6420(3) -0.1608(2) 0.6143(2) 0.0260(8) Uani 1 1 d . . .
C13A C 0.6136(3) -0.09207(19) 0.49831(19) 0.0213(7) Uani 1 1 d . . .
C13 C 0.6181(3) -0.1595(2) 0.5375(2) 0.0266(8) Uani 1 1 d . . .
H13A H 0.6046 -0.2045 0.5105 0.032 Uiso 1 1 calc R . .
N14 N 0.5907(2) -0.09218(16) 0.42287(16) 0.0238(6) Uani 1 1 d . . .
C14B C 0.5633(3) -0.02494(19) 0.30806(18) 0.0211(7) Uani 1 1 d . . .
C14A C 0.5892(2) -0.02745(19) 0.38982(18) 0.0207(7) Uani 1 1 d . . .
C1S C 0.2500 0.0002(8) 0.0000 0.099(4) Uiso 0.90 2 d SPD . 1
Cl1S Cl 0.33941(14) 0.05692(12) -0.03016(11) 0.0772(5) Uani 0.90 1 d PD A 1
Cl2S Cl 0.2707(14) 0.0292(10) -0.0718(5) 0.076(4) Uiso 0.10 1 d PD B 2
C2S C 0.2500 0.0885(16) 0.0000 0.09(3) Uiso 0.10 2 d SPD . 2
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
C1C Re1 C2C 87.84(16) . . ?
C1C Re1 C3C 91.59(19) . . ?
C2C Re1 C3C 87.74(16) . . ?
C1C Re1 N5 174.62(15) . . ?
C2C Re1 N5 96.02(13) . . ?
C3C Re1 N5 92.30(16) . . ?
C1C Re1 N4 100.81(14) . . ?
C2C Re1 N4 170.85(13) . . ?
C3C Re1 N4 94.92(13) . . ?
N5 Re1 N4 75.15(11) . . ?
C1C Re1 Cl1 90.98(14) . . ?
C2C Re1 Cl1 96.44(11) . . ?
C3C Re1 Cl1 175.17(11) . . ?
N5 Re1 Cl1 84.87(8) . . ?
N4 Re1 Cl1 80.58(8) . . ?
O1C C1C Re1 177.7(4) . . ?
O2C C2C Re1 178.4(3) . . ?
O3C C3C Re1 172.5(5) . . ?
C2 C1 C14B 119.0(3) . . ?
C1 C2 C3 119.5(3) . . ?
N4 C3 C2 122.6(3) . . ?
C3 N4 C4A 117.5(3) . . ?
C3 N4 Re1 126.8(2) . . ?
C4A N4 Re1 115.3(2) . . ?
N4 C4A C14B 123.2(3) . . ?
N4 C4A C4B 116.3(3) . . ?
C14B C4A C4B 120.5(3) . . ?
N5 C4B C8A 122.8(3) . . ?
N5 C4B C4A 116.4(3) . . ?
C8A C4B C4A 120.8(3) . . ?
C6 N5 C4B 118.1(3) . . ?
C6 N5 Re1 125.8(2) . . ?
C4B N5 Re1 116.0(2) . . ?
N5 C6 C7 122.2(3) . . ?
C8 C7 C6 119.6(3) . . ?
N9 C8B C14A 122.0(3) . . ?
N9 C8B C8A 117.9(3) . . ?
C14A C8B C8A 120.1(3) . . ?
C4B C8A C8 118.1(3) . . ?
C4B C8A C8B 119.4(3) . . ?
C8 C8A C8B 122.5(3) . . ?
C7 C8 C8A 119.1(3) . . ?
C8B N9 C9A 116.8(3) . . ?
N9 C9A C10 119.9(3) . . ?
N9 C9A C13A 121.2(3) . . ?
C10 C9A C13A 118.9(3) . . ?
C11 C10 C9A 121.3(3) . . ?
C10 C11 C12 120.0(3) . . ?
C10 C11 C11A 120.3(3) . . ?
C12 C11 C11A 119.7(3) . . ?
C13 C12 C11 120.0(3) . . ?
C13 C12 C12A 119.3(3) . . ?
C11 C12 C12A 120.7(3) . . ?
N14 C13A C13 119.8(3) . . ?
N14 C13A C9A 121.2(3) . . ?
C13 C13A C9A 118.9(3) . . ?
C12 C13 C13A 120.8(3) . . ?
C14A N14 C13A 116.7(3) . . ?
C4A C14B C1 118.1(3) . . ?
C4A C14B C14A 119.6(3) . . ?
C1 C14B C14A 122.3(3) . . ?
N14 C14A C8B 122.0(3) . . ?
N14 C14A C14B 118.5(3) . . ?
C8B C14A C14B 119.4(3) . . ?
Cl1S C1S Cl1S 109.6(8) . 2 ?
Cl2S C2S Cl2S 106.0(12) . 2 ?
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 1.918(4) . ?
Re1 C2C 1.929(4) . ?
Re1 C3C 2.006(5) . ?
Re1 N5 2.180(3) . ?
Re1 N4 2.189(3) . ?
Re1 Cl1 2.4755(11) . ?
C1C O1C 1.151(5) . ?
C2C O2C 1.144(5) . ?
C3C O3C 1.021(5) . ?
C1 C2 1.378(5) . ?
C1 C14B 1.398(5) . ?
C2 C3 1.395(5) . ?
C3 N4 1.339(4) . ?
N4 C4A 1.362(4) . ?
C4A C14B 1.393(5) . ?
C4A C4B 1.458(5) . ?
C4B N5 1.356(4) . ?
C4B C8A 1.396(5) . ?
N5 C6 1.345(5) . ?
C6 C7 1.395(5) . ?
C7 C8 1.373(5) . ?
C8B N9 1.331(4) . ?
C8B C14A 1.428(5) . ?
C8B C8A 1.458(5) . ?
C8A C8 1.403(5) . ?
N9 C9A 1.346(4) . ?
C9A C10 1.417(5) . ?
C9A C13A 1.436(5) . ?
C10 C11 1.364(5) . ?
C11 C12 1.436(5) . ?
C11 C11A 1.516(5) . ?
C12A C12 1.509(5) . ?
C12 C13 1.378(5) . ?
C13A N14 1.354(4) . ?
C13A C13 1.417(5) . ?
N14 C14A 1.323(4) . ?
C14B C14A 1.468(4) . ?
C1S Cl1S 1.786(9) . ?
C1S Cl1S 1.786(9) 2 ?
Cl2S C2S 1.788(13) . ?
C2S Cl2S 1.788(13) 2 ?
