Solvent influence on the thermodynamics for hydride transfer from bis(diphosphine) complexes of nickel.
Connelly Robinson, Samantha J.; Zall, Christopher M.; Miller, Deanna L.; Linehan, John C.; Appel, Aaron M.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 10017–10023; doi:10.1039/c6dt00309e

data_7038987
_publ_section_title
;
 Solvent influence on the thermodynamics for hydride transfer from
 bis(diphosphine) complexes of nickel.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10017
_journal_page_last               10023
_journal_paper_doi               10.1039/c6dt00309e
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C20 H32 Ni P4, B F4'
_chemical_formula_sum            'C20 H32 B F4 Ni P4'
_chemical_formula_weight         541.85
_chemical_name_common            Ni(dmpe)2(H)(BF4)
_chemical_name_systematic
'Nickel(II) bis(dimethylphosphinoethane) hydride tetrafluoroborate'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           70
_space_group_name_Hall           '-F 2uv 2vw'
_space_group_name_H-M_alt        'F d d d'
_symmetry_space_group_name_Hall  '-F 2uv 2vw'
_symmetry_space_group_name_H-M   'F d d d :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-03-15 deposited with the CCDC.
2016-04-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.354(3)
_cell_length_b                   19.109(3)
_cell_length_c                   20.927(5)
_cell_measurement_reflns_used    3411
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.720
_cell_measurement_theta_min      2.888
_cell_volume                     4940.3(19)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Olex2 (Dolomanov et al., 2009)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0508
_diffrn_reflns_av_unetI/netI     0.0313
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            13187
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.445
_diffrn_reflns_theta_min         2.191
_exptl_absorpt_coefficient_mu    1.081
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6989
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0557 before and 0.0461 after correction.
The Ratio of minimum to maximum transmission is 0.9376.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_density_diffrn    1.457
_exptl_crystal_description       plate
_exptl_crystal_F_000             2248
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.335
_refine_diff_density_min         -0.235
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     92
_refine_ls_number_reflns         1258
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0506
_refine_ls_R_factor_gt           0.0317
_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^)+(0.0343P)^2^+7.4839P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0687
_refine_ls_wR_factor_ref         0.0743
_reflns_Friedel_coverage         0.000
_reflns_number_gt                977
_reflns_number_total             1258
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt00309e2.cif
_cod_data_source_block           sjc009_0m
_cod_depositor_comments
'Adding full bibliography for 7038986--7038987.cif.'
_cod_original_cell_volume        4940.2(19)
_cod_database_code               7038987
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.938
_shelx_estimated_absorpt_t_max   0.979
_shelx_res_checksum              14447
_solvent_exptl_crystal_recrystallization_method 'acetonitrile, diethyl ether'