The Impact of Hydrogen Bonding on 100% Photo-Switching in Solid-State Nitro-Nitrito Linkage Isomers
Hatcher, Lauren E.; Raithby, Paul R.; CrystEngComm  (2017) –; doi:10.1039/C7CE01366C

data_7229127
_publ_section_title
;
 The Impact of Hydrogen Bonding on 100% Photo-Switching in Solid-State
 Nitro-Nitrito Linkage Isomers
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C7CE01366C
_journal_year                    2017
_chemical_formula_moiety         'C12 H29 N4 O2 Pd, C F3 O3 S'
_chemical_formula_sum            'C13 H29 F3 N4 O5 Pd S'
_chemical_formula_weight         516.86
_chemical_name_systematic
'Nitro(N,N,N,N'-tetraethyldiethylenetriamine)palladium(II) trifluoromethanesulfonate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2017-07-25 deposited with the CCDC.
2017-09-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.782(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.2689(4)
_cell_length_b                   13.0528(5)
_cell_length_c                   16.7054(7)
_cell_measurement_reflns_used    3597
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.8140
_cell_measurement_theta_min      3.9930
_cell_volume                     1997.41(14)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 10.3795
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_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  0.0291
_diffrn_reflns_av_unetI/netI     0.0444
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            8852
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.357
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.092
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81297
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.719
_exptl_crystal_description       block
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.618
_refine_diff_density_min         -0.809
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     270
_refine_ls_number_reflns         4069
_refine_ls_number_restraints     243
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0454
_refine_ls_R_factor_gt           0.0324
_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/[\s^2^(Fo^2^)+(0.0279P)^2^+1.1341P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0661
_refine_ls_wR_factor_ref         0.0716
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3351
_reflns_number_total             4069
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce01366c2.cif
_cod_data_source_block           VT_120K
_cod_database_code               7229127
_shelx_estimated_absorpt_t_min   0.639
_shelx_estimated_absorpt_t_max   0.811
_shelxl_version_number           2014-1
_shelx_res_checksum              5550