Understanding solid-state photoswitching in [Re(OMe2-bpy)(CO)3(η1-NO2)] crystals via in situ photocrystallography
Hatcher, Lauren E.; CrystEngComm 20 (2018) 5990–; doi:10.1039/C8CE00774H

data_7230926
_publ_section_title
;
 Understanding solid-state photoswitching in [Re(OMe2-bpy)(CO)3(\h1-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                   22.7012(19)
_cell_length_b                   22.7012(19)
_cell_length_c                   6.5603(9)
_cell_measurement_reflns_used    907
_cell_measurement_temperature    210(2)
_cell_measurement_theta_max      22.1090
_cell_measurement_theta_min      3.5690
_cell_volume                     3380.8(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      210(2)
_diffrn_detector_area_resol_mean 10.3795
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0995
_diffrn_reflns_av_unetI/netI     0.1852
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            5229
_diffrn_reflns_point_group_measured_fraction_full 0.953
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.313
_diffrn_reflns_theta_min         3.590
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    7.233
_exptl_absorpt_correction_T_max  0.839
_exptl_absorpt_correction_T_min  0.376
_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    2.092
_exptl_crystal_description       needle
_exptl_crystal_F_000             2032
_exptl_crystal_size_max          0.325
_exptl_crystal_size_mid          0.038
_exptl_crystal_size_min          0.025
_refine_diff_density_max         2.367
_refine_diff_density_min         -4.223
_refine_diff_density_rms         0.267
_refine_ls_abs_structure_details
;
 Flack x determined using 374 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.05(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     241
_refine_ls_number_reflns         2958
_refine_ls_number_restraints     264
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.1497
_refine_ls_R_factor_gt           0.0957
_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/[\s^2^(Fo^2^)+(0.0694P)^2^+54.3816P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1880
_refine_ls_wR_factor_ref         0.2319
_reflns_Friedel_coverage         0.746
_reflns_Friedel_fraction_full    0.902
_reflns_Friedel_fraction_max     0.902
_reflns_number_gt                1766
_reflns_number_total             2958
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce00774h2.cif
_cod_data_source_block           PSS_210K
_cod_depositor_comments
'Adding full bibliography for 7230920--7230941.cif.'
_cod_original_cell_volume        3380.8(7)
_cod_database_code               7230926
_shelx_res_checksum              78500