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_1544324
_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         'C29 H34 Co N4 O2 P'
_chemical_formula_sum            'C29 H34 Co N4 O2 P'
_chemical_formula_weight         560.50
_chemical_name_systematic        '[Co(I){(DO)(DOH)pn}(PPh3)]'
_chemical_properties_physical    Air-sensitive,Oxygen-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_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                95.238(1)
_cell_angle_beta                 99.314(1)
_cell_angle_gamma                114.659(1)
_cell_formula_units_Z            2
_cell_length_a                   9.0606(2)
_cell_length_b                   9.2632(2)
_cell_length_c                   18.0169(5)
_cell_measurement_reflns_used    18264
_cell_measurement_temperature    243(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     1334.71(6)
_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  0.0426
_diffrn_reflns_av_unetI/netI     0.0555
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            9429
_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         25.496
_diffrn_reflns_theta_min         2.328
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.737
_exptl_absorpt_correction_T_max  0.964
_exptl_absorpt_correction_T_min  0.916
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Otwinowski et al, 1997'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.395
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             588.0
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   0.964
_exptl_transmission_factor_min   0.916
_refine_diff_density_max         0.353
_refine_diff_density_min         -0.283
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     341
_refine_ls_number_reflns         4937
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0651
_refine_ls_R_factor_gt           0.0437
_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^)+(0.0184P)^2^+0.9820P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0818
_refine_ls_wR_factor_ref         0.0868
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3853
_reflns_number_total             4955
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6fd00210b2.cif
_cod_data_source_block           1
_cod_database_code               1544324
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.916
_shelx_estimated_absorpt_t_max   0.964
_exptl_absorpt_special_details   'Otwinowski et al, 1997'
_shelx_res_checksum              33003
_solvent_exptl_crystal_recrystallization_method Dichloromethane/n-hexane