Structure, magnetism and colour in simple bis(phosphine)nickel(II) dihalide complexes: an experimental and theoretical investigation
Schultz, Madeleine; Plessow, Philipp-Nikolaus; Rominger, Frank; Weigel, Laura; Acta Crystallographica Section C 69 (2013) 1437–1447; doi:10.1107/S0108270113030692

data_2019290
_publ_section_title
;
 Structure, magnetism and colour in simple bis(phosphine)nickel(II)
 dihalide complexes: an experimental and theoretical investigation
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1437
_journal_page_last               1447
_journal_paper_doi               10.1107/S0108270113030692
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          '[Ni I2 (C26 H24 P2)], C H2 Cl2'
_chemical_formula_moiety         'C26 H24 I2 Ni P2, C H2 Cl2'
_chemical_formula_sum            'C27 H26 Cl2 I2 Ni P2'
_chemical_formula_weight         795.83
_chemical_name_systematic
;[1,2-Bis(diphenylphosphanyl)ethane-\k^2^<i>P</i>,<i>P</i>']diiodidonickel(II)
dichloromethane monosolvate
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           110
_space_group_name_Hall           'I 4bw -2c'
_space_group_name_H-M_alt        'I 41 c d'
_symmetry_space_group_name_Hall  'I 4bw -2c'
_symmetry_space_group_name_H-M   'I 41 c d'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   26.3705(17)
_cell_length_b                   26.3705(17)
_cell_length_c                   16.7900(11)
_cell_measurement_reflns_used    9238
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.80
_cell_measurement_theta_min      2.44
_cell_volume                     11675.8(13)
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'SAINT (Bruker, 2005)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008<i>b</i>)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008<i>b</i>)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008<i>b</i>)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008<i>b</i>)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0629
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            109821
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.129
_diffrn_reflns_theta_min         1.544
_exptl_absorpt_coefficient_mu    3.088
_exptl_absorpt_correction_T_max  0.8497
_exptl_absorpt_correction_T_min  0.6521
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Sheldrick, 2008<i>a</i>)
;
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.811
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             6176
_exptl_crystal_size_max          0.330
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.318
_refine_diff_density_min         -1.258
_refine_ls_abs_structure_details
;
Flack x determined using 3206 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons & Flack, 2004)
;
_refine_ls_abs_structure_Flack   -0.004(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         7839
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0426
_refine_ls_R_factor_gt           0.0353
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0204P)^2^+71.4066P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0699
_refine_ls_wR_factor_ref         0.0746
_reflns_number_gt                7131
_reflns_number_total             7839
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fa3325.cif
_cod_data_source_block           lw29
_cod_original_cell_volume        11675.8(17)
_cod_database_code               2019290
_shelx_estimated_absorpt_t_min   0.429
_shelx_estimated_absorpt_t_max   0.861
_shelx_res_checksum              71397
_shelxl_version_number           2.013