Multiple Coordination Geometries Supported by Methylene-Linked Guanidines
Sarah H. Oakley; Martyn P. Coles; Peter B. Hitchcock; Inorganic Chemistry 43 (2004) 7564–7566; doi:10.1021/ic0495416

data_4312111
_publ_section_title
;
 Multiple Coordination Geometries Supported by Methylene-Linked Guanidines
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7564
_journal_page_last               7566
_journal_paper_doi               10.1021/ic0495416
_journal_volume                  43
_journal_year                    2004
_chemical_absolute_configuration ad
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C15 H26 Cl2 Fe1 N6'
_chemical_formula_sum            'C15 H26 Cl2 Fe N6'
_chemical_formula_weight         417.17
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_creation_date             2003-12-04T13:37:03-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 108.886(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.4021(3)
_cell_length_b                   8.2761(3)
_cell_length_c                   12.2393(4)
_cell_measurement_reflns_used    6100
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      3.705
_cell_measurement_wavelength     0.71073
_cell_volume                     901.10(5)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.98
_diffrn_measured_fraction_theta_max 0.98
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.104477
_diffrn_orient_matrix_UB_12      0.377928E-1
_diffrn_orient_matrix_UB_13      0.419802E-1
_diffrn_orient_matrix_UB_21      0.155244E-1
_diffrn_orient_matrix_UB_22      -0.950846E-1
_diffrn_orient_matrix_UB_23      0.529962E-1
_diffrn_orient_matrix_UB_31      0.384689E-1
_diffrn_orient_matrix_UB_32      -0.642688E-1
_diffrn_orient_matrix_UB_33      -0.537208E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0408
_diffrn_reflns_av_unetI/netI     0.0366
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9873
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         4.13
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    1.144
_exptl_absorpt_correction_T_max  0.8455
_exptl_absorpt_correction_T_min  0.7866
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.538
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             436
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.189
_refine_diff_density_min         -0.299
_refine_diff_density_rms         0.044
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.006(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.628
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         3903
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.628
_refine_ls_R_factor_all          0.0262
_refine_ls_R_factor_gt           0.0238
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0777P)^2^+0.6195P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.066
_refine_ls_wR_factor_ref         0.0693
_reflns_number_gt                3746
_reflns_number_total             3903
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0495416si20041014_042851_2.cif
_cod_data_source_block           (3)-dec603
_cod_original_formula_sum        'C15 H26 Cl2 Fe1 N6'
_cod_database_code               4312111