Phosphido complexes derived from 1,1’-ferrocenediyl-bridged secondary diphosphines
Hitzel, Sandra; Färber, Christian; Bruhn, Clemens; Siemeling, Ulrich; Dalton Trans.  (2017) –; doi:10.1039/C7DT00941K

data_7042798
_publ_section_title
;
 Phosphido complexes derived from 1,1&#x2019;-ferrocenediyl-bridged
 secondary diphosphines
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT00941K
_journal_year                    2017
_chemical_formula_moiety         'C54 H46 Fe2 Ni3 P4'
_chemical_formula_sum            'C54 H46 Fe2 Ni3 P4'
_chemical_formula_weight         1106.62
_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   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-03-06 deposited with the CCDC.
2017-04-25 downloaded from the CCDC.
;
_cell_angle_alpha                103.436(19)
_cell_angle_beta                 106.865(19)
_cell_angle_gamma                115.180(18)
_cell_formula_units_Z            1
_cell_length_a                   10.126(3)
_cell_length_b                   11.395(3)
_cell_length_c                   12.124(3)
_cell_measurement_reflns_used    6260
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.87
_cell_measurement_theta_min      1.93
_cell_volume                     1104.6(6)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_details      ' 190 frames, detector distance = 133 mm'
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '1.2, 0.6 mm diameter, multiple pinhole'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  270
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1826
_diffrn_reflns_av_unetI/netI     0.1557
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7162
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.925
_diffrn_source                   'Genix Mo HF'
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    2.080
_exptl_absorpt_correction_T_max  0.8643
_exptl_absorpt_correction_T_min  0.7075
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'X-red ver. 1.58 (Stoe & Cie. 2012)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.664
_exptl_crystal_description       block
_exptl_crystal_F_000             566
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.070
_refine_diff_density_max         1.472
_refine_diff_density_min         -1.396
_refine_diff_density_rms         0.242
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.398
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     286
_refine_ls_number_reflns         3832
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.398
_refine_ls_R_factor_all          0.1853
_refine_ls_R_factor_gt           0.1439
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3669
_refine_ls_wR_factor_ref         0.4285
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2173
_reflns_number_total             3832
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00941k2.cif
_cod_data_source_block           i2175
_cod_original_cell_volume        1104.5(5)
_cod_database_code               7042798
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.719
_shelx_estimated_absorpt_t_max   0.868
_shelx_res_checksum              33843