Synthesis, structure and reactivity of FeII/III-NH3 complexes bearing a tripodal sulfonamido ligand
Nathaniel S. Sickerman; Sonja M. Peterson; Joseph W. Ziller; A. S. Borovik; Chem.Commun. 50 (2014) 2515–; doi:10.1039/c3cc48804g

data_7112029
_publ_section_title
;
 Synthesis, structure and reactivity of FeII/III-NH3 complexes bearing a
 tripodal sulfonamido ligand
;
_journal_name_full               Chem.Commun.
_journal_page_first              2515
_journal_paper_doi               10.1039/c3cc48804g
_journal_volume                  50
_journal_year                    2014
_chemical_absolute_configuration ad
_chemical_formula_sum            'C33 H48 Fe N5 O6 S3'
_chemical_formula_weight         762.79
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      hexagonal
_space_group_IT_number           173
_space_group_name_Hall           'P 6c'
_space_group_name_H-M_alt        'P 63'
_symmetry_space_group_name_Hall  'P 6c'
_symmetry_space_group_name_H-M   'P 63'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   13.6656(9)
_cell_length_b                   13.6656(9)
_cell_length_c                   12.2841(8)
_cell_measurement_reflns_used    9990
_cell_measurement_temperature    88(2)
_cell_measurement_theta_max      28.23
_cell_measurement_theta_min      2.39
_cell_volume                     1986.7(2)
_computing_cell_refinement       'Bruker SAINT 7.68a, 2009'
_computing_data_collection       'Bruker APEX2 2011.4-1, 2011'
_computing_data_reduction        'Bruker SAINT 7.68a, 2009'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'Bruker SHELXTL 2008/4'
_diffrn_ambient_temperature      88(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0246
_diffrn_reflns_av_unetI/netI     0.0195
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            23645
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.278
_diffrn_reflns_theta_min         1.721
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.583
_exptl_absorpt_correction_T_max  0.9721
_exptl_absorpt_correction_T_min  0.8556
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Bruker SADABS 2008/1'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    not_measured
_exptl_crystal_description       hexagon
_exptl_crystal_F_000             806
_exptl_crystal_size_max          0.294
_exptl_crystal_size_mid          0.178
_exptl_crystal_size_min          0.134
_refine_diff_density_max         0.316
_refine_diff_density_min         -0.256
_refine_diff_density_rms         0.041
_refine_ls_abs_structure_details
; 
 Flack x determined using 1459 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons and Flack (2004), Acta Cryst. A60, s61). 
;
_refine_ls_abs_structure_Flack   0.025(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     149
_refine_ls_number_reflns         3279
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0233
_refine_ls_R_factor_gt           0.0221
_refine_ls_shift/su_max          0.026
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0399P)^2^+0.1507P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0611
_refine_ls_wR_factor_ref         0.0616
_reflns_Friedel_coverage         0.900
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.985
_reflns_number_gt                3176
_reflns_number_total             3279
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3cc48804g.txt
_cod_data_source_block           asb240
_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 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        1986.7(3)
_cod_database_code               7112029
_shelx_estimated_absorpt_t_min   0.847
_shelx_estimated_absorpt_t_max   0.926
_shelxl_version_number           2013-3
_shelx_res_checksum              14954
_shelx_hkl_checksum              42492
_shelx_fab_checksum              79842