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_1544325
_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         'C24 H32 Co N4 O2 P'
_chemical_formula_sum            'C24 H32 Co N4 O2 P'
_chemical_formula_weight         498.44
_chemical_name_systematic        '[Co(I){(DO)(DOH)pn}(PMePh2)]'
_chemical_properties_physical    Air-sensitive,Oxygen-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-06-02 deposited with the CCDC.
2016-10-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.0720(2)
_cell_length_b                   17.0259(3)
_cell_length_c                   18.8998(3)
_cell_measurement_reflns_used    65603
_cell_measurement_temperature    243(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     4849.96(13)
_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  0.0796
_diffrn_reflns_av_unetI/netI     0.0331
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            33617
_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         25.500
_diffrn_reflns_theta_min         2.102
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.802
_exptl_absorpt_correction_T_max  0.921
_exptl_absorpt_correction_T_min  0.758
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Otwinowski et al, 1997'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.365
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2096.0
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.08
_exptl_transmission_factor_max   0.921
_exptl_transmission_factor_min   0.758
_refine_diff_density_max         0.898
_refine_diff_density_min         -0.504
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     297
_refine_ls_number_reflns         4519
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0720
_refine_ls_R_factor_gt           0.0475
_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^)+(0.0436P)^2^+4.9676P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1022
_refine_ls_wR_factor_ref         0.1105
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3410
_reflns_number_total             4521
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6fd00210b2.cif
_cod_data_source_block           2
_cod_database_code               1544325
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.758
_shelx_estimated_absorpt_t_max   0.921
_exptl_absorpt_special_details   'Otwinowski et al, 1997'
_shelx_res_checksum              88740
_solvent_exptl_crystal_recrystallization_method Dichloromethane/n-hexane