Tuning low-coordinate metal environments: high spin d5‒d7 complexes supported by bis(phosphinimino)methyl ligation
Evans, David J.; Hill, Michael S.; Hitchcock, Peter B.; Dalton Transactions  (2003) 570–; doi:10.1039/b210467a

data_7012375
_publ_section_title
;
 Tuning low-coordinate metal environments: high spin d5--d7 complexes
 supported by bis(phosphinimino)methyl ligation
;
_journal_issue                   4
_journal_name_full               'Dalton Transactions'
_journal_page_first              570
_journal_paper_doi               10.1039/b210467a
_journal_year                    2003
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C49 H61 Fe N3 P2 Si2'
_chemical_formula_sum            'C49 H61 Fe N3 P2 Si2'
_chemical_formula_weight         865.98
_chemical_name_common            '[Fe{N(SiMe3)2}{MesNPPh2CHPPh2NMes}]'
_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_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             2002-04-08T11:40:56-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 94.420(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.9774(3)
_cell_length_b                   18.4685(4)
_cell_length_c                   21.5940(7)
_cell_measurement_reflns_used    13569
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      22.986
_cell_measurement_theta_min      3.705
_cell_measurement_wavelength     0.71073
_cell_volume                     4762.5(2)
_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_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.82311E-1
_diffrn_orient_matrix_UB_12      0.98156E-2
_diffrn_orient_matrix_UB_13      0.20774E-2
_diffrn_orient_matrix_UB_21      0.107199E-1
_diffrn_orient_matrix_UB_22      -0.299292E-1
_diffrn_orient_matrix_UB_23      0.385919E-1
_diffrn_orient_matrix_UB_31      0.110597E-1
_diffrn_orient_matrix_UB_32      -0.440422E-1
_diffrn_orient_matrix_UB_33      -0.257624E-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  0.0783
_diffrn_reflns_av_unetI/netI     0.0533
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            24917
_diffrn_reflns_theta_full        23.04
_diffrn_reflns_theta_max         23.04
_diffrn_reflns_theta_min         3.72
_exptl_absorpt_coefficient_mu    0.47
_exptl_absorpt_correction_T_max  0.971
_exptl_absorpt_correction_T_min  0.907
_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    1.208
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1840
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.242
_refine_diff_density_min         -0.287
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.06
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     528
_refine_ls_number_reflns         6580
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.06
_refine_ls_R_factor_all          0.0743
_refine_ls_R_factor_gt           0.049
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0368P)^2^+5.2924P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0998
_refine_ls_wR_factor_ref         0.1115
_reflns_number_gt                5041
_reflns_number_total             6580
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b210467a.txt
_cod_data_source_block           apr202
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7012375