Nickel complexes of a binucleating ligand derived from an SCS pincer.
Peterson, Sonja M.; Helm, Monte L.; Appel, Aaron M.; Dalton transactions (Cambridge, England : 2003) 44 (2015) 747–752; doi:10.1039/c4dt02718c

data_7033106
_publ_section_title
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 Nickel complexes of a binucleating ligand derived from an SCS pincer.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              747
_journal_page_last               752
_journal_paper_doi               10.1039/c4dt02718c
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C16 H23 Br Ni O3 S2'
_chemical_formula_sum            'C16 H23 Br Ni O3 S2'
_chemical_formula_weight         466.08
_chemical_name_systematic        NiLBr
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2013-08-26
_audit_creation_method
;
  Olex2 1.2
  (compiled 2013.03.22 svn.r2654, GUI svn.r4446)
;
_cell_angle_alpha                90
_cell_angle_beta                 95.684(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   8.5902(3)
_cell_length_b                   16.4831(6)
_cell_length_c                   25.1988(11)
_cell_measurement_reflns_used    9735
_cell_measurement_temperature    140
_cell_measurement_theta_max      28.36
_cell_measurement_theta_min      2.60
_cell_volume                     3550.4(2)
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      140
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0414
_diffrn_reflns_av_unetI/netI     0.0559
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            34120
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.781
_diffrn_reflns_theta_min         2.471
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.589
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9015
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0733 before and 0.0606 after correction.
The Ratio of minimum to maximum transmission is 0.9015.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.744
_exptl_crystal_description       block
_exptl_crystal_F_000             1904
_exptl_crystal_size_max          0.085
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.539
_refine_diff_density_min         -0.466
_refine_diff_density_rms         0.079
_refine_ls_abs_structure_details
;
 Flack x determined using 3294 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.027(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.959
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         9056
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.959
_refine_ls_R_factor_all          0.0426
_refine_ls_R_factor_gt           0.0300
_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^)+(0.0120P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0459
_refine_ls_wR_factor_ref         0.0486
_reflns_Friedel_coverage         0.957
_reflns_Friedel_fraction_full    0.984
_reflns_Friedel_fraction_max     0.957
_reflns_number_gt                7623
_reflns_number_total             9056
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt02718c2.cif
_cod_data_source_block           helm136_0m
_cod_depositor_comments
'Adding full bibliography for 7033106--7033107.cif.'
_cod_database_code               7033106
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C25(H25A,H25B), C9(H9A,H9B), C11(H11A,H11B), C27(H27A,H27B),
 C30(H30A,H30B), C32(H32A,H32B), C26(H26A,H26B), C12(H12A,H12B), C10(H10A,H10B),
  C16(H16A,H16B), C15(H15A,H15B), C3(H3A,H3B), C29(H29A,H29B), C28(H28A,H28B),
 C19(H19A,H19B), C31(H31A,H31B), C24(H24A,H24B), C14(H14A,H14B), C13(H13A,H13B)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C20(H20), C6(H6), C22(H22), C5(H5), C21(H21)
;
_shelx_estimated_absorpt_t_max   0.870
_shelx_estimated_absorpt_t_min   0.750
_shelx_hkl_checksum              34255
_shelx_res_checksum              16278
_shelxl_version_number           2013-2