Turning a New Leaf on Metal-TMC Chemistry: Ni(II)(TMC) Acetylides.
Tyler, Sarah F.; Natoli, Sean N.; Vlaisavljevich, Bess; Fanwick, Phillip E.; Ren, Tong; Inorganic chemistry 54 (2015) 10058–10064; doi:10.1021/acs.inorgchem.5b01883

data_4346649
_publ_section_title
;
 Turning a New Leaf on Metal-TMC Chemistry: Ni(II)(TMC) Acetylides.
;
_journal_issue                   20
_journal_name_full               'Inorganic chemistry'
_journal_page_first              10058
_journal_page_last               10064
_journal_paper_doi               10.1021/acs.inorgchem.5b01883
_journal_volume                  54
_journal_year                    2015
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C18 H33 N4 Ni1,C1 F3 O3 S1'
_chemical_formula_sum            'C19 H33 F3 N4 Ni O3 S'
_chemical_formula_weight         513.26
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.7849(8)
_cell_length_b                   8.3978(4)
_cell_length_c                   14.8663(5)
_cell_measurement_reflns_used    9703
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      72.305
_cell_measurement_theta_min      5.771
_cell_volume                     2345.19(17)
_computing_cell_refinement       'HKL3000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'Crystal Clear(Rigaku 2001)'
_computing_data_reduction        'HKL3000 (Otwinowski & Minor, 1997)'
_computing_publication_material  'local programs'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.940
_diffrn_measured_fraction_theta_max 0.914
_diffrn_measurement_details
;
Data were collected on a Rigaku Rapid which has a quarter 
chi circle and a 200 degree curved image plate at a fixed 
distance of 127.4mm.  Strategy was optimized using the 
CrystalClear software.  The completeness is the best 
that can be obtained with this geometry. The missing data are not 
cusp data but mostly high angle data.
Also the use of HKL3000/SCALEPACK lowers the number 
of observed data as inconsistent equivalents are removed 
from the data set and not included in the collected total.
;
_diffrn_measurement_device_type  'Rigaku Rapid II'
_diffrn_measurement_method       \w
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.000
_diffrn_reflns_av_unetI/netI     0.0531
_diffrn_reflns_Laue_measured_fraction_max 0.914
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9703
_diffrn_reflns_point_group_measured_fraction_full 0.942
_diffrn_reflns_point_group_measured_fraction_max 0.916
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.305
_diffrn_reflns_theta_min         5.771
_diffrn_source                   'microfocus source'
_exptl_absorpt_coefficient_mu    2.483
_exptl_absorpt_correction_T_max  0.905
_exptl_absorpt_correction_T_min  0.323
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.454
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.475
_refine_diff_density_min         -0.347
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.02(4)
_refine_ls_extinction_coef       0.0027(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.142
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     286
_refine_ls_number_reflns         3740
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.141
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0397
_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^)+(0.0631P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1064
_refine_ls_wR_factor_ref         0.1214
_reflns_Friedel_coverage         0.923
_reflns_Friedel_fraction_full    0.944
_reflns_Friedel_fraction_max     0.918
_reflns_number_gt                3112
_reflns_number_total             3740
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01883_si_002.cif
_cod_data_source_block           SFT3
_cod_database_code               4346649
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              15096
_shelx_hkl_checksum              80350