Extended Network Thiocyanate- and Tetracyanoethanide-Based First-Row Transition Metal Complexes
Endrit Shurdha; Saul H. Lapidus; Peter W. Stephens; Curtis E. Moore; Arnold L. Rheingold; Joel S. Miller; Inorganic Chemistry 51 (2012) 9655–9665; doi:10.1021/ic300804y

data_4330311
_publ_contact_author_address
; 
Department of Chemistry
University of Utah
Salt Lake City
UT 84112-0850
USA 
;
_publ_contact_author_email       JSMILLER@chem.utah.edu
_publ_contact_author_name        'Joel S. Miller'
_publ_section_title
;
 Extended Network Thiocyanate- and Tetracyanoethanide-Based First-Row
 Transition Metal Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9655
_journal_page_last               9665
_journal_paper_doi               10.1021/ic300804y
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C8 H12 Mn N2 O2 S2'
_chemical_formula_weight         287.26
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_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
_cell_angle_alpha                110.69(3)
_cell_angle_beta                 99.104(16)
_cell_angle_gamma                97.89(3)
_cell_formula_units_Z            1
_cell_length_a                   5.801(8)
_cell_length_b                   7.874(10)
_cell_length_c                   8.036(12)
_cell_measurement_reflns_used    1046
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.70
_cell_measurement_theta_min      2.78
_cell_volume                     331.6(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.912
_diffrn_measured_fraction_theta_max 0.811
_diffrn_measurement_device_type  'Bruker APEX CCD'
_diffrn_measurement_method       '\f scans'
_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  0.0972
_diffrn_reflns_av_sigmaI/netI    0.0667
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            1628
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.15
_diffrn_reflns_theta_min         2.78
_exptl_absorpt_coefficient_mu    1.293
_exptl_absorpt_correction_T_max  0.6749
_exptl_absorpt_correction_T_min  0.6393
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.439
_exptl_crystal_description       block
_exptl_crystal_F_000             147
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.33
_refine_diff_density_max         0.984
_refine_diff_density_min         -0.490
_refine_diff_density_rms         0.146
_refine_ls_extinction_coef       0.17(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     73
_refine_ls_number_reflns         1317
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0666
_refine_ls_R_factor_gt           0.0635
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1152P)^2^+0.3144P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1736
_refine_ls_wR_factor_ref         0.1774
_reflns_number_gt                1187
_reflns_number_total             1317
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic300804y_si_002_9.cif
_cod_data_source_block           jsm152
_cod_database_code               4330311