Reversible Cooperative Dihydrogen Binding and Transfer with a Bis-Phosphenium Complex of Chromium
Birchall, Nicholas; Feil, Christoph M.; Gediga, Michael; Nieger, Martin; Gudat, Dietrich; Chemical Science  (2020) –; doi:10.1039/D0SC03773G

data_1558894
_publ_section_title
;
 Reversible Cooperative Dihydrogen Binding and Transfer with a
 Bis-Phosphenium Complex of Chromium
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D0SC03773G
_journal_year                    2020
_chemical_formula_moiety         'C57 H77 Cr N5 O3 P2, C55 H74 Cr N4 O3 P2'
_chemical_formula_sum            'C112 H151 Cr2 N9 O6 P4'
_chemical_formula_weight         1947.29
_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'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2020-05-26 deposited with the CCDC.	2020-08-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.6854(10)
_cell_length_b                   20.8290(9)
_cell_length_c                   40.6993(18)
_cell_measurement_reflns_used    8413
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      1.0
_cell_volume                     21774.2(16)
_computing_cell_refinement       'Bruker ApexII Software Suite, 2008'
_computing_data_collection       'Bruker ApexII Software Suite, 2008'
_computing_data_reduction        'Bruker ApexII Software Suite, 2008'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    SHELXS-86
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Kappa ApexII Duo'
_diffrn_measurement_method       'Omega and phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2791
_diffrn_reflns_av_unetI/netI     0.1843
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            170081
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.382
_diffrn_reflns_theta_min         1.277
_diffrn_source                   'fine focus sealed tube'
_exptl_absorpt_coefficient_mu    0.314
_exptl_absorpt_correction_T_max  0.7152
_exptl_absorpt_correction_T_min  0.6897
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.188
_exptl_crystal_description       blcoks
_exptl_crystal_F_000             8336
_exptl_crystal_size_max          0.122
_exptl_crystal_size_mid          0.121
_exptl_crystal_size_min          0.081
_refine_diff_density_max         0.776
_refine_diff_density_min         -0.411
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.979
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1190
_refine_ls_number_reflns         19979
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      0.979
_refine_ls_R_factor_all          0.2201
_refine_ls_R_factor_gt           0.0827
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1721
_refine_ls_wR_factor_ref         0.2301
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8413
_reflns_number_total             19979
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc03773g2.cif
_cod_data_source_block           g523_mn
_cod_database_code               1558894
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.963
_shelx_estimated_absorpt_t_max   0.975
_shelx_res_checksum              92457