Unusual stability of dyads during photochemical hydrogen production.
Prock, J.; Strabler, C.; Viertl, W.; Kopacka, H.; Obendorf, D.; Müller, T; Tordin, E.; Salzl, S.; Knör, G; Mauro, M.; De Cola, L.; Brüggeller, P; Dalton transactions (Cambridge, England : 2003) 44 (2015) 20936–20948; doi:10.1039/c5dt03414k

data_7037143
_publ_section_title
;
 Unusual stability of dyads during photochemical hydrogen production.
;
_journal_issue                   48
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              20936
_journal_page_last               20948
_journal_paper_doi               10.1039/c5dt03414k
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         '2(C82 H68 N6 Os P4 Pd), 8(F6 P), 5(C2 H3 N)'
_chemical_formula_sum            'C174 H151 F48 N17 Os2 P16 Pd2'
_chemical_formula_weight         4480.91
_chemical_melting_point_gt       573
_chemical_name_systematic        '[Os(bpy)2(dppcb)Pd(bpy)](PF6)4'
_chemical_properties_physical    'Light-sensitive, Photo-sensitive'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-06-03 deposited with the CCDC.
2015-11-10 downloaded from the CCDC.
;
_cell_angle_alpha                72.7270(8)
_cell_angle_beta                 88.1416(9)
_cell_angle_gamma                89.5445(8)
_cell_formula_units_Z            1
_cell_length_a                   14.0903(2)
_cell_length_b                   17.9570(3)
_cell_length_c                   20.4371(3)
_cell_measurement_reflns_used    200095
_cell_measurement_temperature    243(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     4935.17(13)
_computing_cell_refinement       'Denzo and Scalepack'
_computing_data_collection       'Kappa CCD'
_computing_data_reduction        'Denzo and Scalepack'
_computing_molecular_graphics    'SHELXTL-NT V6.1'
_computing_publication_material  'SHELXTL-NT V6.1'
_computing_structure_refinement  'SHELXL-2015 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      243(2)
_diffrn_measured_fraction_theta_full 1.00
_diffrn_measurement_device_type  'Kappa CCD'
_diffrn_measurement_method       'phi- and omega-scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0243
_diffrn_reflns_av_sigmaI/netI    0.0488
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            40080
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         1.99
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.690
_exptl_absorpt_correction_T_max  0.765
_exptl_absorpt_correction_T_min  0.475
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Otwinowski et al, 1997'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.508
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2230
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Acetonitrile'
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.310
_refine_diff_density_min         -0.820
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1192
_refine_ls_number_reflns         22419
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0532
_refine_ls_R_factor_gt           0.0437
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0749P)^2^+4.4469P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1241
_refine_ls_wR_factor_ref         0.1424
_reflns_number_gt                17732
_reflns_number_total             22745
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt03414k2.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' tag was changed to
'_chemical_melting_point_gt' since the value was specified 'more
than' ('>') a certain temperature. The value '> 573' was changed to
'573' - it should be numeric and without a unit designator.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 7037143--7037145.cif.
;
_cod_database_code               7037143
_diffrn_measured_fraction        0.997