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_4346647
_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_formula_moiety         'C25 H51 N4 Ni1 Si1,Cl1,2(H2 O1)'
_chemical_formula_sum            'C25 H55 Cl N4 Ni O2 Si'
_chemical_formula_weight         565.98
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 111.638(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   43.9611(17)
_cell_length_b                   9.0601(4)
_cell_length_c                   17.3189(7)
_cell_measurement_reflns_used    26311
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      67.816
_cell_measurement_theta_min      4.328
_cell_volume                     6411.9(5)
_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 (Sheldrick, 2014)'
_computing_structure_solution    'SIR2004 (Burla, et. al., 2005)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_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  0.060
_diffrn_reflns_av_unetI/netI     0.0315
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       52
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            26311
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         67.816
_diffrn_reflns_theta_min         4.328
_diffrn_source                   'microfocus source'
_exptl_absorpt_coefficient_mu    2.190
_exptl_absorpt_correction_T_max  0.916
_exptl_absorpt_correction_T_min  0.135
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.173
_exptl_crystal_description       platelet
_exptl_crystal_F_000             2464
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.643
_refine_diff_density_min         -0.478
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     351
_refine_ls_number_reflns         5694
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0735
_refine_ls_R_factor_gt           0.0630
_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^)+(0.1017P)^2^+11.6858P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1798
_refine_ls_wR_factor_ref         0.1910
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4669
_reflns_number_total             5694
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01883_si_002.cif
_cod_data_source_block           SFT1
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4346647
_shelx_estimated_absorpt_t_min   0.621
_shelx_estimated_absorpt_t_max   0.918
_shelxl_version_number           2014-3
_shelx_res_checksum              39576
_shelx_hkl_checksum              60081