#------------------------------------------------------------------------------
#$Date: 2019-11-23 22:19:22 +0200 (Sat, 23 Nov 2019) $
#$Revision: 235336 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/62/7236271.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_7236271
loop_
_publ_author_name
'Świtlicka, Anna'
'Klemens, Tomasz'
'Machura, Barbara'
'Schab-Balcerzak, Ewa'
'Laba, Katarzyna'
'Lapkowski, Mieczyslaw'
'Grucela, Marzena'
'Nycz, Jacek'
'Szala, Marcin'
'Kania, Magdalena'
_publ_section_title
;
 Rhenium(i) complexes with phenanthrolines bearing electron-withdrawing Cl
 and electron-donating CH3 substituents -- synthesis, photophysical,
 thermal, and electrochemical properties with electroluminescence ability
;
_journal_issue                   114
_journal_name_full               'RSC Advances'
_journal_page_first              112908
_journal_paper_doi               10.1039/C6RA23935H
_journal_volume                  6
_journal_year                    2016
_chemical_formula_moiety         'C17 H10 Cl2 N3 O3 Re'
_chemical_formula_sum            'C17 H10 Cl2 N3 O3 Re'
_chemical_formula_weight         561.38
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2016-08-31 deposited with the CCDC.
2016-11-30 downloaded from the CCDC.
;
_cell_angle_alpha                84.319(3)
_cell_angle_beta                 85.261(3)
_cell_angle_gamma                67.529(4)
_cell_formula_units_Z            2
_cell_length_a                   8.3105(3)
_cell_length_b                   9.7851(4)
_cell_length_c                   12.3202(5)
_cell_measurement_reflns_used    3961
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      27.7720
_cell_measurement_theta_min      4.0820
_cell_volume                     920.16(7)
_computing_cell_refinement       'CrysAlis RED v. 1.163 (UNIL IC & KUMA 2000)'
_computing_data_collection       'CrysAlis CCD v. 1.163 (UNIL IC & KUMA 2000)'
_computing_data_reduction        'CrysAlis RED v. 1.163 (UNIL IC & KUMA 2000)'
_computing_molecular_graphics
'Mercury (Macrae, J.Appl.Cryst. 41 (2008) 466-470'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Oxford Diffraction Gemini A Ultra'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0479
_diffrn_reflns_av_unetI/netI     0.0606
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7649
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.048
_diffrn_reflns_theta_min         3.883
_exptl_absorpt_coefficient_mu    6.915
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.36218
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, Acta Cryst. A51 (1995) 33-38'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.026
_exptl_crystal_description       plate
_exptl_crystal_F_000             532
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.762
_refine_diff_density_min         -1.000
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.971
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         3248
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.971
_refine_ls_R_factor_all          0.0404
_refine_ls_R_factor_gt           0.0298
_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)+(0.0119P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0484
_refine_ls_wR_factor_ref         0.0512
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2795
_reflns_number_total             3248
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6ra23935h2.cif
_cod_data_source_block           ren4120
_cod_database_code               7236271
_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.
;
_shelxl_version_number           2014/6
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -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
Re1 Re 0.64014(2) 0.71041(2) 0.69907(2) 0.03442(8) Uani 1 1 d . .
N1 N 0.5403(5) 0.7904(4) 0.8576(4) 0.0313(10) Uani 1 1 d . .
N2 N 0.8726(4) 0.6717(4) 0.7886(4) 0.0313(10) Uani 1 1 d . .
N3 N 0.9643(7) 0.9980(7) 0.7900(6) 0.0763(18) Uani 1 1 d . .
O3 O 0.6391(6) 1.0041(5) 0.5882(4) 0.0763(14) Uani 1 1 d . .
O1 O 0.8040(6) 0.5648(6) 0.4883(5) 0.0891(16) Uani 1 1 d . .
O2 O 0.2867(5) 0.7769(5) 0.6039(4) 0.0747(14) Uani 1 1 d . .
Cl1 Cl 0.65176(15) 0.47083(13) 0.79392(13) 0.0443(3) Uani 1 1 d . .
Cl2 Cl 0.7062(2) 0.79698(17) 1.25009(14) 0.0619(4) Uani 1 1 d . .
C3 C 0.6385(6) 0.8936(7) 0.6317(5) 0.0477(15) Uani 1 1 d . .
C1 C 0.7449(7) 0.6195(6) 0.5696(6) 0.0534(16) Uani 1 1 d . .
C2 C 0.4196(7) 0.7490(6) 0.6393(5) 0.0440(14) Uani 1 1 d . .
C4 C 0.3710(6) 0.8463(5) 0.8927(5) 0.0376(13) Uani 1 1 d . .
H4 H 0.2861 0.8644 0.8427 0.045 Uiso 1 1 calc R U
C5 C 0.3184(6) 0.8778(5) 1.0000(5) 0.0383(13) Uani 1 1 d . .
H5 H 0.2002 0.9178 1.0201 0.046 Uiso 1 1 calc R U
C6 C 0.4392(6) 0.8504(5) 1.0766(5) 0.0412(13) Uani 1 1 d . .
H6 H 0.4042 0.8693 1.1491 0.049 Uiso 1 1 calc R U
C7 C 0.6177(6) 0.7930(5) 1.0437(5) 0.0324(12) Uani 1 1 d . .
C8 C 0.7584(7) 0.7649(5) 1.1143(5) 0.0381(13) Uani 1 1 d . .
C9 C 0.9265(6) 0.7123(5) 1.0774(5) 0.0401(14) Uani 1 1 d . .
H9 H 1.0140 0.6967 1.1250 0.048 Uiso 1 1 calc R U
C10 C 0.9714(6) 0.6804(5) 0.9662(5) 0.0328(12) Uani 1 1 d . .
C11 C 1.1451(6) 0.6191(5) 0.9235(5) 0.0397(14) Uani 1 1 d . .
H11 H 1.2374 0.6001 0.9680 0.048 Uiso 1 1 calc R U
C12 C 1.1762(6) 0.5885(5) 0.8173(5) 0.0426(15) Uani 1 1 d . .
H12 H 1.2902 0.5497 0.7883 0.051 Uiso 1 1 calc R U
C13 C 1.0374(6) 0.6149(5) 0.7513(5) 0.0410(13) Uani 1 1 d . .
H13 H 1.0611 0.5921 0.6788 0.049 Uiso 1 1 calc R U
C14 C 0.8388(6) 0.7034(5) 0.8945(5) 0.0304(12) Uani 1 1 d . .
C15 C 0.6614(5) 0.7629(5) 0.9347(4) 0.0300(11) Uani 1 1 d . .
C16 C 0.9331(10) 1.1671(8) 0.6153(7) 0.089(2) Uani 1 1 d . .
H16A H 1.0351 1.1277 0.5679 0.133 Uiso 1 1 calc R U
H16B H 0.9200 1.2642 0.6333 0.133 Uiso 1 1 calc R U
H16C H 0.8323 1.1735 0.5790 0.133 Uiso 1 1 calc R U
C17 C 0.9508(8) 1.0716(8) 0.7132(7) 0.0595(18) 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'
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
C1 Re1 C3 89.2(3)
C1 Re1 C2 87.1(2)
C3 Re1 C2 89.7(2)
C1 Re1 N1 173.1(2)
C3 Re1 N1 96.2(2)
C2 Re1 N1 97.22(19)
C1 Re1 N2 100.2(2)
C3 Re1 N2 92.79(18)
C2 Re1 N2 172.3(2)
N1 Re1 N2 75.28(14)
C1 Re1 Cl1 92.07(19)
C3 Re1 Cl1 177.26(16)
C2 Re1 Cl1 92.83(16)
N1 Re1 Cl1 82.37(10)
N2 Re1 Cl1 84.58(10)
C4 N1 C15 116.6(5)
C4 N1 Re1 126.4(3)
C15 N1 Re1 116.3(3)
C13 N2 C14 118.7(4)
C13 N2 Re1 127.0(4)
C14 N2 Re1 114.2(3)
O3 C3 Re1 178.4(6)
O1 C1 Re1 177.6(5)
O2 C2 Re1 177.8(5)
N1 C4 C5 122.9(5)
C6 C5 C4 120.5(5)
C5 C6 C7 118.8(5)
C15 C7 C6 117.7(5)
C15 C7 C8 117.5(4)
C6 C7 C8 124.8(5)
C9 C8 C7 122.0(5)
C9 C8 Cl2 120.2(4)
C7 C8 Cl2 117.8(4)
C8 C9 C10 120.6(5)
C14 C10 C11 116.9(5)
C14 C10 C9 119.6(4)
C11 C10 C9 123.5(5)
C12 C11 C10 119.6(5)
C11 C12 C13 120.0(5)
N2 C13 C12 122.2(5)
N2 C14 C10 122.6(4)
N2 C14 C15 118.6(4)
C10 C14 C15 118.8(5)
N1 C15 C7 123.5(4)
N1 C15 C14 114.9(5)
C7 C15 C14 121.5(4)
N3 C17 C16 179.5(8)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Re1 C1 1.884(7)
Re1 C3 1.895(6)
Re1 C2 1.919(5)
Re1 N1 2.158(4)
Re1 N2 2.191(4)
Re1 Cl1 2.4848(13)
N1 C4 1.351(6)
N1 C15 1.373(6)
N2 C13 1.326(6)
N2 C14 1.353(6)
N3 C17 1.117(9)
O3 C3 1.160(6)
O1 C1 1.165(7)
O2 C2 1.144(6)
Cl2 C8 1.722(6)
C4 C5 1.383(7)
C5 C6 1.368(7)
C6 C7 1.411(6)
C7 C15 1.393(7)
C7 C8 1.440(7)
C8 C9 1.347(7)
C9 C10 1.422(7)
C10 C14 1.406(6)
C10 C11 1.413(7)
C11 C12 1.353(8)
C12 C13 1.394(7)
C14 C15 1.428(6)
C16 C17 1.432(11)
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C4 H4 N3 0.93 2.59 3.425(8) 149.0 1_455
C12 H12 Cl1 0.93 2.81 3.664(5) 153.7 1_655
C16 H16C O2 0.96 2.47 3.269(9) 141.2 2_676
C6 H6 Cl2 0.93 2.71 3.072(6) 104.3 .
