Stabilisation effects of phosphane ligands in the homogeneous approach of sunlight induced hydrogen production
Brueggeller, Peter; Strabler, Christof; Sinn, Stephan; Pehn, Richard; Pann, Johann; Dutzler, Julian; Viertl, Wolfgang; Prock, Johannes; Ehrmann, Katharina; Weninger, Alexander; Kopacka, Holger; De Cola, Luisa; Faraday Discuss.  (2016) –; doi:10.1039/C6FD00210B

data_1544326
_publ_section_title
;
 Stabilisation effects of phosphane ligands in the homogeneous approach of
 sunlight induced hydrogen production
;
_journal_name_full               'Faraday Discuss.'
_journal_paper_doi               10.1039/C6FD00210B
_journal_year                    2016
_chemical_formula_moiety
'C97 H82 N4 Os P6 Pd, 4(F6 P), 1.12(C Cl2), 1.42(C Cl), 1.42(Cl)'
_chemical_formula_sum            'C99.54 H82 Cl5.08 F24 N4 Os P10 Pd'
_chemical_formula_weight         2576.59
_chemical_name_systematic        '[Os(bpy)2(dppcb)Pd(dppm)](PF6)4'
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yac'
_space_group_name_H-M_alt        'P 1 n 1'
_symmetry_space_group_name_Hall  'P -2yac'
_symmetry_space_group_name_H-M   'P 1 n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-08-31 deposited with the CCDC.
2016-10-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.3398(8)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.6742(3)
_cell_length_b                   13.9310(2)
_cell_length_c                   24.3295(4)
_cell_measurement_reflns_used    211818
_cell_measurement_temperature    243(2)
_cell_measurement_theta_max      26.022
_cell_measurement_theta_min      0.998
_cell_volume                     5718.15(16)
_computing_cell_refinement       'Denzo and Scalepack'
_computing_data_collection       'Kappa CCD'
_computing_data_reduction        'Denzo and Scalepack'
_computing_molecular_graphics    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      243(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Kappa CCD'
_diffrn_measurement_method       'phi- and omega-scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0349
_diffrn_reflns_av_unetI/netI     0.0662
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            20704
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.249
_diffrn_reflns_theta_min         1.705
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.609
_exptl_absorpt_correction_T_max  0.845
_exptl_absorpt_correction_T_min  0.740
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Otwinowski et al, 1997'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.497
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2563.2
_exptl_crystal_preparation       ', Luminescent'
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_exptl_transmission_factor_max   0.845
_exptl_transmission_factor_min   0.740
_refine_diff_density_max         0.602
_refine_diff_density_min         -0.673
_refine_diff_density_rms         0.085
_refine_ls_abs_structure_details
; 
 Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F^2^, conventional R-factors R are based 
 on F, with F set to zero for negative F^2^. The threshold expression of 
 F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F^2^ are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.581(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1352
_refine_ls_number_reflns         19865
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0890
_refine_ls_R_factor_gt           0.0580
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0609P)^2^+10.9763P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1184
_refine_ls_wR_factor_ref         0.1295
_reflns_Friedel_coverage         0.999
_reflns_Friedel_fraction_full    0.993
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                15563
_reflns_number_total             20704
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6fd00210b2.cif
_cod_data_source_block           1
_cod_database_code               1544326
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.740
_shelx_estimated_absorpt_t_max   0.845
_exptl_absorpt_special_details   'Otwinowski et al, 1997'
_shelx_res_checksum              56789