Hydrogen-Bonding Motifs in MS2N2H Metallacycles: A Crystallographic and Computational Study of [CpCoS2N2H][BF4]
Boeré, René T.; Crystal Growth & Design 14 (2014) 814–; doi:10.1021/cg401674w

data_4509885
_publ_section_title
;
 Hydrogen-Bonding Motifs in MS2N2H Metallacycles: A Crystallographic and
 Computational Study of [CpCoS2N2H][BF4]
;
_journal_issue                   2
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              814
_journal_paper_doi               10.1021/cg401674w
_journal_volume                  14
_journal_year                    2014
_chemical_formula_moiety         'C5 H6 Co N2 S2, B F4'
_chemical_formula_sum            'C5 H6 B Co F4 N2 S2'
_chemical_formula_weight         303.98
_chemical_melting_point          383
_chemical_name_common
;
 [CpCoS2N2H][BF4]
;
_chemical_name_systematic
; 
 N2-5-(eta-5-Cyclopentadienyl)-5-cobalta-1,3,2,4-dithiadiazolium
 tetrafluoroborate 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.264(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   14.587(3)
_cell_length_b                   7.6483(13)
_cell_length_c                   18.132(3)
_cell_measurement_reflns_used    3984
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.12
_cell_measurement_theta_min      2.86
_cell_volume                     1976.7(6)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2008)'
_computing_data_collection       'APEX2 (Bruker, 2008)'
_computing_data_reduction        SAINT-Plus
_computing_molecular_graphics    'Mercury (Macrae <i>et al.</i>, 2006)'
_computing_publication_material  'publCIF (Westrip, 2007)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_diffrn_ambient_pressure         101
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
;
 Bruker ApexII CCD area-detector diffractometer
;
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1184
_diffrn_reflns_av_unetI/netI     0.0956
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            19617
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.250
_diffrn_reflns_theta_max         26.010
_diffrn_reflns_theta_min         1.632
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Bruker D8'
_exptl_absorpt_coefficient_mu    2.180
_exptl_absorpt_correction_T_max  0.9785
_exptl_absorpt_correction_T_min  0.5009
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
SADABS (Bruker, 2006)
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.043
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1200
_exptl_crystal_recrystallization_method 'Slow cooling'
_exptl_crystal_size_max          0.368
_exptl_crystal_size_mid          0.145
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.318
_refine_diff_density_min         -0.959
_refine_diff_density_rms         0.127
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     279
_refine_ls_number_reflns         3886
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.1209
_refine_ls_R_factor_gt           0.0577
_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^)+(0.0575P)^2^+3.2435P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1194
_refine_ls_wR_factor_ref         0.1452
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2255
_reflns_number_total             3886
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cg401674w_si_002.cif
_cod_data_source_block           CpCoS2N2HBF4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_Hall     -P2yn
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4509885
_shelx_estimated_absorpt_t_min   0.501
_shelx_estimated_absorpt_t_max   0.979