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_2242703
_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_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_formula_moiety         'C52 H48 Ni P4, 2(C F3 O3 S)'
_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(diphenylphosphino)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
_audit_creation_date             2018-04-26
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90
_cell_angle_beta                 97.996(13)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.984(8)
_cell_length_b                   16.087(12)
_cell_length_c                   14.375(10)
_cell_measurement_reflns_used    3687
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      22.797
_cell_measurement_theta_min      2.510
_cell_volume                     2515(3)
_computing_cell_refinement       'Bruker SAINT (Bruker, 2013)'
_computing_data_collection       'Bruker APEX2 (Bruker, 2013)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2013)'
_computing_molecular_graphics
;Bruker SHELXTL (Bruker, 2013), 
 Mercury v3.9 (Macrae et al., 2006)
;
_computing_publication_material
;
publCIF v1.9.21_c (Westrip, 2010), 
Olex2 (Dolomanov et al., 2009)
;
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0638
_diffrn_reflns_av_unetI/netI     0.0634
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            29647
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.248
_diffrn_reflns_theta_min         1.910
_diffrn_source                   'fine-focus X-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.670
_exptl_absorpt_correction_T_max  0.958
_exptl_absorpt_correction_T_min  0.872
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.523
_exptl_crystal_density_method    'Not measured'
_exptl_crystal_description       Cube
_exptl_crystal_F_000             1188
_exptl_crystal_size_max          0.211
_exptl_crystal_size_mid          0.128
_exptl_crystal_size_min          0.065
_refine_diff_density_max         0.497
_refine_diff_density_min         -0.478
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     404
_refine_ls_number_reflns         6535
_refine_ls_number_restraints     133
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.1098
_refine_ls_R_factor_gt           0.0565
_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^)+(0.0496P)^2^+2.3473P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1149
_refine_ls_wR_factor_ref         0.1478
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3880
_reflns_number_total             6535
_reflns_threshold_expression     'I > 2\s(I)'
_publcif_datablock.id            {ba89ee9d-f4c6-4e37-8ebb-b09bb48d4894}
_cod_data_source_file            hb7775sup3.txt
_cod_data_source_block           1_296K
_cod_database_code               2242703
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.7457
_shelx_estimated_absorpt_t_min   0.6852
_shelx_res_checksum              308
_shelx_hkl_checksum              27684