Raising the (metastable) bar: 100% photo-switching in [Pd(Bu4dien)(η1-N̲O2)]+approaches ambient temperature
Hatcher, Lauren E.; CrystEngComm 18 (2016) 4180–; doi:10.1039/C5CE02434J

data_7224224
_publ_section_title
;
 Raising the (metastable) bar: 100% photo-switching in
 [Pd(Bu4dien)(\h1-N&#x0332;O2)]+approaches ambient temperature
;
_journal_issue                   22
_journal_name_full               CrystEngComm
_journal_page_first              4180
_journal_paper_doi               10.1039/C5CE02434J
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety
;
C20 H45 N4 O2 Pd, C24 H20 B, C4 H8 O
;
_chemical_formula_sum            'C48 H73 B N4 O3 Pd'
_chemical_formula_weight         871.31
_chemical_name_systematic
'Nitro-(N,N,N',N'-tetrabutyldiethylenetriamine)palladium(II)tetraphenylborate, tetrahydrofuran solvate'
_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'
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_atom_sites_solution_hydrogens   mixed
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_audit_update_record
;
2015-12-10 deposited with the CCDC.
2016-02-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.725(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
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_cell_measurement_reflns_used    3033
_cell_measurement_temperature    260(2)
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_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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_computing_molecular_graphics
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ORTEP-3 (Farrugia, 2012)
MERCURY (MCarae 2008)
;
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2015)'
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_diffrn_ambient_temperature      260(2)
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_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0727
_diffrn_reflns_av_unetI/netI     0.1318
_diffrn_reflns_Laue_measured_fraction_full 0.998
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_diffrn_reflns_limit_h_max       14
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_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            20892
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_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         3.006
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.434
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86609
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Rigaku-Oxford Diffraction,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.222
_exptl_crystal_description       Needle
_exptl_crystal_F_000             1856
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.459
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_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.983
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     509
_refine_ls_number_reflns         9671
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.983
_refine_ls_R_factor_all          0.1492
_refine_ls_R_factor_gt           0.0601
_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^)+(0.0346P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0904
_refine_ls_wR_factor_ref         0.1157
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5082
_reflns_number_total             9671
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce02434j2.cif
_cod_data_source_block           SS-260K
_cod_depositor_comments
'Adding full bibliography for 7224206--7224224.cif.'
_cod_database_code               7224224
_shelx_estimated_absorpt_t_min   0.930
_shelx_estimated_absorpt_t_max   0.987
_shelxl_version_number           2014-1
_shelx_res_checksum              36194