Crystal structure at 100K of bis[1,2-bis(diphenylphosphanyl)ethane]nickel(II) bis(trifluoromethanesulfonate): a possible negative thermal expansion molecular material
Cano-Benítez, Cristian A.; Metta-Magaña, Alejandro J.; Duarte-Ruiz, Álvaro; Acta Crystallographica Section E 74 (2018) 1678–1681; doi:10.1107/S2056989018014846

data_2242702
_publ_section_title
;
 Crystal structure at 100K of
 bis[1,2-bis(diphenylphosphanyl)ethane]nickel(II)
 bis(trifluoromethanesulfonate): a possible negative thermal expansion
 molecular material
;
_journal_coeditor_code           HB7775
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1678
_journal_page_last               1681
_journal_paper_doi               10.1107/S2056989018014846
_journal_volume                  74
_journal_year                    2018
_chemical_compound_source        Synthesis
_chemical_formula_iupac          '[Ni (C26 H24 P2)2] (C F3 O3 S)2'
_chemical_formula_moiety         'C52 H48 Ni P4 2+, 2(C S O3 F3-)'
_chemical_formula_sum            'C54 H48 F6 Ni O6 P4 S2'
_chemical_formula_weight         1153.63
_chemical_name_common            'bis(dppe))nickel(II) bis(triflate)'
_chemical_name_systematic
;
Bis[1,2-bis(diphenylphosphanyl)ethane]nickel(II)
bis(trifluoromethanesulfonate)
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     other
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 98.1430(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.0462(4)
_cell_length_b                   16.1813(6)
_cell_length_c                   14.3914(5)
_cell_measurement_reflns_used    8190
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.902
_cell_measurement_theta_min      2.248
_cell_volume                     2546.41(16)
_computing_cell_refinement
;
SAINT (Bruker, 2013)
;
_computing_data_collection
;
APEX2 (Bruker, 2013)
;
_computing_data_reduction
;
SAINT (Bruker, 2013)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008) and Mercury (Macrae <i>et al.</i>,
2006)
;
_computing_publication_material
;
publCIF (Westrip, 2010) and <i>OLEX2</i> (Dolomanov <i>et al.</i>,
2009)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_av_unetI/netI     0.0388
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            30965
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.959
_diffrn_reflns_theta_min         1.905
_diffrn_source                   'fine-focus X-ray tube'
_exptl_absorpt_coefficient_mu    0.662
_exptl_absorpt_correction_T_max  0.974
_exptl_absorpt_correction_T_min  0.828
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2013)
;
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.505
_exptl_crystal_density_method    'Not measured'
_exptl_crystal_description       Cube
_exptl_crystal_F_000             1188
_exptl_crystal_size_max          0.205
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.094
_refine_diff_density_max         0.637
_refine_diff_density_min         -0.304
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     395
_refine_ls_number_reflns         7253
_refine_ls_number_restraints     144
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0538
_refine_ls_R_factor_gt           0.0402
_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^)+(0.0417P)^2^+1.7778P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0886
_refine_ls_wR_factor_ref         0.0989
_reflns_number_gt                5928
_reflns_number_total             7253
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            hb7775sup1.cif
_cod_data_source_block           I
_cod_database_code               2242702
_cod_database_fobs_code          2242702
_shelx_estimated_absorpt_t_min   0.876
_shelx_estimated_absorpt_t_max   0.940
_shelx_hkl_checksum              61604
_shelx_res_checksum              52159
_shelxl_version_number           2014/6