Structure and Polymorphism in M(ethylenediamine)3MoS4(M = Mn, Co, Ni)
Tian, Hengfeng; Iliff, Hadley A.; Moore, Lee J.; Oertel, Catherine M.; Crystal Growth & Design 10 (2010) 669–; doi:10.1021/cg901087x

data_4502382
_publ_contact_author
; Dr Catherine M. Oertel
Department of Chemistry and Biochemistry
Oberlin College 
Oberlin, OH  44074, USA 
;
_publ_section_title
;
 Structure and Polymorphism in M(ethylenediamine)3MoS4(M = Mn, Co, Ni)
;
_journal_issue                   2
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              669
_journal_paper_doi               10.1021/cg901087x
_journal_volume                  10
_journal_year                    2010
_chemical_formula_moiety         'C6 H24 N6 Ni, Mo S4'
_chemical_formula_sum            'C6 H24 Mo N6 Ni S4'
_chemical_formula_weight         463.20
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.916(13)
_cell_length_b                   7.610(3)
_cell_length_c                   14.093(6)
_cell_measurement_reflns_used    1672
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.46
_cell_measurement_theta_min      2.90
_cell_volume                     1707.0(17)
_computing_cell_refinement       'APEX2 v2008.2-4'
_computing_data_collection       'APEX2 v2008.2-4 (Bruker, 2008)'
_computing_data_reduction        'APEX2 v2008.2-4'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker AXS SMART APEX CCD diffractometer'
_diffrn_measurement_method       '\w 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  0.0442
_diffrn_reflns_av_sigmaI/netI    0.0537
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            8523
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.56
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.320
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.6451
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Apex2 v2008.2-4 (Bruker, 2008)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.802
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.040
_refine_diff_density_max         1.114
_refine_diff_density_min         -0.595
_refine_diff_density_rms         0.117
_refine_ls_abs_structure_details
'Flack H D (1983), Acta Cryst. A39, 876-881, 1036 pairs'
_refine_ls_abs_structure_Flack   0.016(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         3224
_refine_ls_number_restraints     33
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_gt           0.0344
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0240P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0613
_refine_ls_wR_factor_ref         0.0662
_reflns_number_gt                2759
_reflns_number_total             3224
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            cg901087x_si_001.cif
_cod_data_source_block           a-Ni(en)3MoS4_(1)
_cod_original_sg_symbol_Hall     P2c-2n
_cod_original_sg_symbol_H-M      Pna21
_cod_database_code               4502382
_publ_section_refinement
; Absolute configuration was determined using the 
Flack parameter with 1036 Freidel pairs.  H atoms 
were refined using a riding model, employing HFIX in SHELX.  
C-H distances were fixed at 0.99 angstroms and N-H 
distances at 0.92 angstroms.  DELU and SIMU commands were 
applied to the disordered C1 and C2 atoms.
;