#------------------------------------------------------------------------------
#$Date: 2019-11-17 08:57:38 +0200 (Sun, 17 Nov 2019) $
#$Revision: 228978 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/09/7230928.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_7230928
loop_
_publ_author_name
'Hatcher, Lauren E.'
_publ_section_title
;
 Understanding solid-state photoswitching in [Re(OMe2-bpy)(CO)3(η1-NO2)]
 crystals via in situ photocrystallography
;
_journal_issue                   39
_journal_name_full               CrystEngComm
_journal_page_first              5990
_journal_paper_doi               10.1039/C8CE00774H
_journal_volume                  20
_journal_year                    2018
_chemical_formula_moiety         'C15 H12 N3 O7 Re'
_chemical_formula_sum            'C15 H12 N3 O7 Re'
_chemical_formula_weight         532.48
_chemical_name_systematic
;
Nitro-(4,4'-dimethoxy-2,2'-bipyridine)-rhenium(I)-tricarbonyl
;
_chemical_properties_physical    Light-sensitive,Photo-sensitive
_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_Hall           'I -4'
_space_group_name_H-M_alt        'I -4'
_symmetry_space_group_name_Hall  'I -4'
_symmetry_space_group_name_H-M   'I -4'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2018-05-11 deposited with the CCDC.
2018-06-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.738(2)
_cell_length_b                   22.738(2)
_cell_length_c                   6.5434(9)
_cell_measurement_reflns_used    2221
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.7440
_cell_measurement_theta_min      3.5570
_cell_volume                     3383.0(6)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2015)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 10.3795
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0804
_diffrn_reflns_av_unetI/netI     0.1081
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            5957
_diffrn_reflns_point_group_measured_fraction_full 0.936
_diffrn_reflns_point_group_measured_fraction_max 0.933
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.336
_diffrn_reflns_theta_min         2.833
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    7.228
_exptl_absorpt_correction_T_max  0.878
_exptl_absorpt_correction_T_min  0.817
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.091
_exptl_crystal_description       needle
_exptl_crystal_F_000             2032
_exptl_crystal_size_max          0.288
_exptl_crystal_size_mid          0.023
_exptl_crystal_size_min          0.019
_refine_diff_density_max         2.442
_refine_diff_density_min         -1.991
_refine_diff_density_rms         0.222
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.04(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         2899
_refine_ls_number_restraints     259
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0774
_refine_ls_R_factor_gt           0.0641
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0902P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1559
_refine_ls_wR_factor_ref         0.1663
_reflns_Friedel_coverage         0.707
_reflns_Friedel_fraction_full    0.861
_reflns_Friedel_fraction_max     0.855
_reflns_number_gt                2461
_reflns_number_total             2899
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8ce00774h2.cif
_cod_data_source_block           PSS_200K
_cod_depositor_comments
'Adding full bibliography for 7230920--7230941.cif.'
_cod_original_cell_volume        3383.0(8)
_cod_database_code               7230928
_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.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'y, -x, -z'
'-x, -y, z'
'-y, x, -z'
'x+1/2, y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.5977(11) 0.3224(11) -0.003(4) 0.031(3) Uani 1 1 d . U . . .
C2 C 0.5518(11) 0.3597(11) 0.358(4) 0.035(3) Uani 1 1 d . U . . .
C3 C 0.4905(11) 0.3702(11) 0.007(4) 0.030(4) Uani 1 1 d . U . . .
C4 C 0.4280(11) 0.3025(12) 0.479(4) 0.031(4) Uani 1 1 d . U . . .
H4 H 0.4474 0.3351 0.5325 0.037 Uiso 1 1 calc R U . . .
C5 C 0.3787(10) 0.2816(11) 0.579(4) 0.031(4) Uani 1 1 d . U . . .
H5 H 0.3642 0.3010 0.6938 0.037 Uiso 1 1 calc R U . . .
C6 C 0.3513(10) 0.2312(11) 0.507(3) 0.025(4) Uani 1 1 d . U . . .
C7 C 0.3713(9) 0.2074(10) 0.324(3) 0.025(4) Uani 1 1 d . U . . .
H7 H 0.3516 0.1757 0.2659 0.030 Uiso 1 1 calc R U . . .
C8 C 0.4186(10) 0.2297(10) 0.231(3) 0.022(3) Uani 1 1 d . U . . .
C9 C 0.4435(10) 0.2073(10) 0.041(4) 0.026(4) Uani 1 1 d . U . . .
C10 C 0.4195(13) 0.1576(13) -0.064(4) 0.040(6) Uani 1 1 d . U . . .
H10 H 0.3870 0.1378 -0.0115 0.048 Uiso 1 1 calc R U . . .
C11 C 0.4454(12) 0.1395(11) -0.243(4) 0.029(4) Uani 1 1 d . U . . .
C12 C 0.4924(11) 0.1697(10) -0.318(4) 0.031(4) Uani 1 1 d . U . . .
H12 H 0.5100 0.1581 -0.4399 0.038 Uiso 1 1 calc R U . . .
C13 C 0.5138(12) 0.2175(11) -0.212(3) 0.031(4) Uani 1 1 d . U . . .
H13 H 0.5465 0.2372 -0.2631 0.038 Uiso 1 1 calc R U . . .
C14 C 0.2813(13) 0.2316(15) 0.775(4) 0.052(8) Uani 1 1 d . U . . .
H14A H 0.3120 0.2358 0.8748 0.078 Uiso 1 1 calc R U . . .
H14B H 0.2506 0.2073 0.8302 0.078 Uiso 1 1 calc R U . . .
H14C H 0.2656 0.2697 0.7425 0.078 Uiso 1 1 calc R U . . .
C15 C 0.4451(16) 0.0699(16) -0.517(5) 0.067(10) Uani 1 1 d . U . . .
H15A H 0.4833 0.0533 -0.4926 0.100 Uiso 1 1 calc R U . . .
H15B H 0.4484 0.1017 -0.6124 0.100 Uiso 1 1 calc R U . . .
H15C H 0.4195 0.0402 -0.5716 0.100 Uiso 1 1 calc R U . . .
N2 N 0.4492(9) 0.2779(9) 0.306(3) 0.027(2) Uani 1 1 d . U . . .
N3 N 0.4894(9) 0.2362(9) -0.041(3) 0.030(2) Uani 1 1 d . U . . .
O3 O 0.6409(8) 0.3339(8) -0.081(3) 0.047(5) Uani 1 1 d . U . . .
O4 O 0.5651(10) 0.3909(10) 0.479(3) 0.056(6) Uani 1 1 d . U . . .
O5 O 0.4677(10) 0.4057(10) -0.080(3) 0.060(6) Uani 1 1 d . U . . .
O6 O 0.3047(8) 0.2049(9) 0.594(2) 0.042(4) Uani 1 1 d . U . . .
O7 O 0.4215(9) 0.0913(9) -0.329(3) 0.052(5) Uani 1 1 d . U . . .
Re1 Re 0.52751(4) 0.30529(4) 0.14819(14) 0.0289(3) Uani 1 1 d . U . . .
N1 N 0.575(2) 0.226(2) 0.298(9) 0.035(3) Uani 0.36(2) 1 d D U P A 1
O1 O 0.560(2) 0.1765(18) 0.269(7) 0.035(3) Uani 0.36(2) 1 d D U P A 1
O2 O 0.616(2) 0.235(2) 0.409(8) 0.035(3) Uani 0.36(2) 1 d D U P A 1
N1A N 0.6043(12) 0.2169(11) 0.376(6) 0.035(3) Uani 0.64(2) 1 d D U P A 2
O1A O 0.5548(11) 0.2278(13) 0.287(5) 0.035(3) Uani 0.64(2) 1 d D U P A 2
O2A O 0.6366(11) 0.2633(11) 0.397(4) 0.035(3) Uani 0.64(2) 1 d D U P A 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'
Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 -1 0 0.0116
1 1 1 0.1206
-1 -1 -1 0.1391
-1 1 0 0.0116
-1 -1 0 0.0096
1 1 0 0.0096
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
O3 C1 Re1 175(2)
O4 C2 Re1 179(3)
O5 C3 Re1 176(2)
N2 C4 C5 123(2)
C4 C5 C6 119(2)
O6 C6 C5 125(2)
O6 C6 C7 117(2)
C5 C6 C7 118(2)
C8 C7 C6 121(2)
C7 C8 N2 123(2)
C7 C8 C9 125(2)
N2 C8 C9 113(2)
N3 C9 C10 119(2)
N3 C9 C8 118(2)
C10 C9 C8 123(2)
C11 C10 C9 119(2)
O7 C11 C12 125(2)
O7 C11 C10 115(2)
C12 C11 C10 119(3)
C11 C12 C13 120(2)
N3 C13 C12 122(2)
C4 N2 C8 116(2)
C4 N2 Re1 125.3(17)
C8 N2 Re1 118.2(15)
C13 N3 C9 121(2)
C13 N3 Re1 123.3(17)
C9 N3 Re1 115.5(16)
C6 O6 C14 117(2)
C11 O7 C15 119(2)
C1 Re1 C2 90.0(11)
C1 Re1 C3 87.8(10)
C2 Re1 C3 88.5(11)
C1 Re1 O1A 98.6(11)
C2 Re1 O1A 98.4(11)
C3 Re1 O1A 170.5(11)
C1 Re1 N2 174.6(10)
C2 Re1 N2 94.6(9)
C3 Re1 N2 95.1(9)
O1A Re1 N2 77.9(10)
C1 Re1 N3 100.5(9)
C2 Re1 N3 168.7(9)
C3 Re1 N3 96.0(9)
O1A Re1 N3 76.0(10)
N2 Re1 N3 74.7(8)
C1 Re1 N1 89.2(18)
C2 Re1 N1 93.5(14)
C3 Re1 N1 176.3(19)
N2 Re1 N1 87.7(16)
N3 Re1 N1 82.5(12)
O2 N1 O1 118(6)
O2 N1 Re1 120(4)
O1 N1 Re1 122(4)
O1A N1A O2A 113(3)
N1A O1A Re1 128(2)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
C1 O3 1.14(3)
C1 Re1 1.92(2)
C2 O4 1.10(3)
C2 Re1 1.93(3)
C3 O5 1.12(3)
C3 Re1 1.93(2)
C4 N2 1.35(3)
C4 C5 1.38(3)
C5 C6 1.39(3)
C6 O6 1.34(3)
C6 C7 1.39(3)
C7 C8 1.34(3)
C8 N2 1.39(3)
C8 C9 1.45(3)
C9 N3 1.35(3)
C9 C10 1.43(4)
C10 C11 1.38(4)
C11 O7 1.35(3)
C11 C12 1.36(3)
C12 C13 1.38(3)
C13 N3 1.32(3)
C14 O6 1.44(3)
C15 O7 1.43(3)
N2 Re1 2.151(19)
N3 Re1 2.18(2)
Re1 O1A 2.08(3)
Re1 N1 2.32(5)
N1 O2 1.197(14)
N1 O1 1.198(14)
N1A O1A 1.290(13)
N1A O2A 1.294(13)
