Selective coordination of cyanate and thiocyanate in the end-on mode: synthesis, structures and properties of [NiII2L(μ1,1-NCO)]+ and [NiII2L(μ1,1-NCS)]+ (L2− = macrocyclic N6S2 ligand)
Jeremies, Alexander; Gruschinski, Sina; Schmorl, Sara; Severin, Tobias; Kersting, Berthold; New Journal of Chemistry 42 (2018) 7630–; doi:10.1039/C8NJ00114F

data_7057185
_publ_section_title
;
 Selective coordination of cyanate and thiocyanate in the end-on mode:
 synthesis, structures and properties of [NiII2L(\m1,1-NCO)]+ and
 [NiII2L(\m1,1-NCS)]+ (L2&#x2212; = macrocyclic N6S2 ligand)
;
_journal_issue                   10
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              7630
_journal_paper_doi               10.1039/C8NJ00114F
_journal_volume                  42
_journal_year                    2018
_chemical_formula_sum            'C62.33 H84 B N6.34 Ni2 O S2'
_chemical_formula_weight         1130.42
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2018-01-08 deposited with the CCDC.
2018-03-19 downloaded from the CCDC.
;
_cell_angle_alpha                76.17(3)
_cell_angle_beta                 67.57(3)
_cell_angle_gamma                88.95(3)
_cell_formula_units_Z            2
_cell_length_a                   13.419(3)
_cell_length_b                   15.603(3)
_cell_length_c                   16.433(3)
_cell_measurement_reflns_used    13600
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      56.0
_cell_measurement_theta_min      6.0
_cell_volume                     3078.0(14)
_computing_cell_refinement       'STOE IPDS software'
_computing_data_collection       'STOE IPDS software'
_computing_data_reduction        'STOE X-AREA'
_computing_molecular_graphics    ORTEP-III
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.906
_diffrn_measured_fraction_theta_max 0.906
_diffrn_measurement_device_type  'STOE IPDS-1'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0969
_diffrn_reflns_av_sigmaI/netI    0.1825
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            44836
_diffrn_reflns_theta_full        28.20
_diffrn_reflns_theta_max         28.20
_diffrn_reflns_theta_min         2.62
_exptl_absorpt_coefficient_mu    0.724
_exptl_absorpt_correction_T_max  0.8992
_exptl_absorpt_correction_T_min  0.8122
_exptl_absorpt_process_details
;
Busing, W. R. & Levy, H. A. (1957) Acta Cryst. 10, 180-182. 
and  
Coppens, P., Leiserowitz, L. & Rabinovich, D. (1965) 
Acta Cryst. 1965, 1035-1038.
;
_exptl_crystal_colour            bright-green
_exptl_crystal_density_diffrn    1.220
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1207
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_platon_squeeze_details
;
;
_refine_diff_density_max         0.420
_refine_diff_density_min         -0.383
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.663
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     704
_refine_ls_number_reflns         13738
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      0.664
_refine_ls_R_factor_all          0.1252
_refine_ls_R_factor_gt           0.0455
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0242P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0752
_refine_ls_wR_factor_ref         0.0903
_reflns_number_gt                5560
_reflns_number_total             13738
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8nj00114f2.cif
_cod_data_source_block           ocn24sq
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7057185.cif.
;
_cod_original_cell_volume        3078.1(11)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7057185