1,2-Bis(diphenylphosphino)ethane nickel(ii) O,O′-dialkyldithiophosphates as potential precursors for nickel sulfides
Yadav, Reena; Singh, Ashish Kumar; Waghadkar, Yogesh; Kociok-Köhn, Gabriele; Kumar, Abhinav; Chauhan, Ratna; Rane, Sunit; Gosavi, Suresh; New J. Chem. 41 (2017) 1327–; doi:10.1039/C6NJ03186B

data_7055917
_publ_section_title
;
 1,2-Bis(diphenylphosphino)ethane nickel(ii)
 O,O&#x2032;-dialkyldithiophosphates as potential precursors for nickel
 sulfides
;
_journal_issue                   3
_journal_name_full               'New J. Chem.'
_journal_page_first              1327
_journal_paper_doi               10.1039/C6NJ03186B
_journal_volume                  41
_journal_year                    2017
_chemical_formula_moiety
'2(C32 H38 Ni O2 P3 S2), 2(C24 H20 B), 0.5(C H2 Cl2)'
_chemical_formula_sum            'C112.5 H117 B2 Cl Ni2 O4 P6 S4'
_chemical_formula_weight         2021.60
_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
;
2016-10-05 deposited with the CCDC.
2016-12-21 downloaded from the CCDC.
;
_cell_angle_alpha                102.5046(7)
_cell_angle_beta                 101.1188(7)
_cell_angle_gamma                106.1991(7)
_cell_formula_units_Z            1
_cell_length_a                   11.9740(2)
_cell_length_b                   14.1021(2)
_cell_length_c                   17.2015(4)
_cell_measurement_reflns_used    107634
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.910
_cell_volume                     2621.90(9)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
;
 DENZO-SCALEPACK Z. Otwinowski and W. Minor, " 
 Processing of X-ray Diffraction Data Collected in Oscillation Mode ", 
 Methods in Enzymology, Volume 276: Macromolecular Crystallography, 
 part A, p.307-326, 1997,C.W. Carter, Jr. & R. M. Sweet, Eds., Academic Press.
;
_computing_molecular_graphics
'ORTEP3 for Windows - Farrugia, L. J. J. Appl. Crystallogr. 1997, 30, 565'
_computing_publication_material
;
 'WinGX publication routines, Farrugia, 
 L. J., J. Appl. Crystallogr., 1999, 32, 837-838
;
_computing_structure_refinement
;
 SHELXL-2014/7 (Sheldrick, 2014)
 Sheldrick GM (2008) Acta Crystallogr A64:112--122 and 
 C. B. H\"ubschle, G. M. Sheldrick and B. Dittrich
 ShelXle: a Qt graphical user interface for SHELXL
 J. Appl. Cryst., 44, (2011) 1281-1284.
;
_computing_structure_solution
; 
 SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , 
 Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. 
 (1999) J. Appl. Cryst. 32, 115-119
;
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       '387 1.4 degree images with \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0581
_diffrn_reflns_av_unetI/netI     0.0471
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            53581
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         3.485
_exptl_absorpt_coefficient_mu    0.607
_exptl_absorpt_correction_T_max  0.897
_exptl_absorpt_correction_T_min  0.732
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_description       prism
_exptl_crystal_F_000             1061
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.300
_refine_diff_density_max         0.359
_refine_diff_density_min         -0.391
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     617
_refine_ls_number_reflns         11899
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0660
_refine_ls_R_factor_gt           0.0452
_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^)+(0.0262P)^2^+2.5686P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0963
_refine_ls_wR_factor_ref         0.1034
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9369
_reflns_number_total             11899
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6nj03186b2.cif
_cod_data_source_block           k14gkk8
_cod_depositor_comments
'Adding full bibliography for 7055917--7055919.cif.'
_cod_original_cell_volume        2621.90(8)
_cod_original_formula_sum        'C112.50 H117 B2 Cl Ni2 O4 P6 S4'
_cod_database_code               7055917
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.751
_shelx_estimated_absorpt_t_max   0.839
_shelx_res_checksum              22074