Ni(ii) complexes of the phosphine-oxime Ph<sub>2</sub>PC<sub>6</sub>H<sub>4</sub>-2-CH[double bond, length as m-dash]NOH.
Basu, Debashis; Woods, Toby J.; Rauchfuss, Thomas B.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 7256–7262; doi:10.1039/c8dt01551a

data_7046264
_publ_section_title
;
 Ni(ii) complexes of the phosphine-oxime
 Ph<sub>2</sub>PC<sub>6</sub>H<sub>4</sub>-2-CH[double bond, length as
 m-dash]NOH.
;
_journal_issue                   21
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7256
_journal_page_last               7262
_journal_paper_doi               10.1039/c8dt01551a
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C57 H45 N3 Ni3 O4 P3, B F4, 0.5(H2 O)'
_chemical_formula_sum            'C57 H46 B F4 N3 Ni3 O4.5 P3'
_chemical_formula_weight         1200.82
_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
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-04-04 deposited with the CCDC.
2018-05-08 downloaded from the CCDC.
;
_cell_angle_alpha                91.309(3)
_cell_angle_beta                 108.166(3)
_cell_angle_gamma                118.187(3)
_cell_formula_units_Z            2
_cell_length_a                   14.4858(13)
_cell_length_b                   14.8932(13)
_cell_length_c                   15.1803(12)
_cell_measurement_reflns_used    51757
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.55
_cell_measurement_theta_min      2.38
_cell_volume                     2685.6(4)
_computing_cell_refinement       'SAINT V8.34A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2014.9-0 (Bruker, 2014)'
_computing_data_reduction
; 
SAINT V8.34A, XPREP v2014/2, TWINABS V2012/1 
(Bruker, 2012 & 2014) 
;
_computing_molecular_graphics
; 
SHELXTL v2014-7 (Bruker, 2014), CrystalMaker v2.7.7 (CrystalMaker, 1994) 
;
_computing_publication_material  'XCIF V2014-2 (Bruker, 2014)'
_computing_structure_refinement  'SHELX-2014-7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT-2014-4 (Sheldrick, 2015b)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device       'Bruker D8 Venture/Photon 100'
_diffrn_measurement_method       'profile data from \f and \w scans'
_diffrn_radiation_monochromator  'multilayer mirrors'
_diffrn_radiation_source         'microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  twin4_a_sq
_diffrn_reflns_av_R_equivalents  0.0361
_diffrn_reflns_av_unetI/netI     0.0530
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18684
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.540
_diffrn_reflns_theta_min         2.349
_exptl_absorpt_coefficient_mu    1.195
_exptl_absorpt_correction_T_max  0.745209
_exptl_absorpt_correction_T_min  0.642095
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS V2014/5 (Bruker, 2014)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.485
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate-like
_exptl_crystal_F_000             1230
_exptl_crystal_id                twin4_a_sq
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) with the (1 2 0) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.298
_exptl_crystal_size_mid          0.051
_exptl_crystal_size_min          0.042
_platon_squeeze_details
; 
One void space containing significant electron density was identified 
by SQUEEZE. The electron density removed from this void space is consistent 
with two methanol solvate molecules, making the most probable solution one 
that consists of one methanol molecule per target molecule.
;
_refine_diff_density_max         0.700
_refine_diff_density_min         -0.675
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.134
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     688
_refine_ls_number_reflns         9844
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.134
_refine_ls_R_factor_all          0.0719
_refine_ls_R_factor_gt           0.0540
_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^)+(0.0166P)^2^+10.2153P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1021
_refine_ls_wR_factor_ref         0.1080
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8288
_reflns_number_total             9844
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01551a2.cif
_cod_data_source_block           twin4_a_sq
_cod_depositor_comments
'Adding full bibliography for 7046263--7046270.cif.'
_cod_original_formula_sum        'C57 H46 B F4 N3 Ni3 O4.50 P3'
_cod_database_code               7046264
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.717
_shelx_estimated_absorpt_t_max   0.952
_shelx_res_checksum              94678
_shelx_fab_checksum              32742
_platon_squeeze_void_probe_radius 1.20