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_7012377
_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_formula_sum            'C62 H58 Fe N2 O P2'
_chemical_formula_weight         964.89
_chemical_name_common            '[Fe(OCPh3)(MesNPPh2CHPPh2NMes)]'
_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_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             2002-05-13T10:53:04-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                92.801(1)
_cell_angle_beta                 92.638(1)
_cell_angle_gamma                107.006(1)
_cell_formula_units_Z            2
_cell_length_a                   10.4976(2)
_cell_length_b                   12.7168(2)
_cell_length_c                   19.7847(4)
_cell_measurement_reflns_used    14433
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      3.705
_cell_volume                     2517.64(8)
_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_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0564
_diffrn_reflns_av_unetI/netI     0.0771
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            24791
_diffrn_reflns_theta_full        27.5
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         3.77
_exptl_absorpt_coefficient_mu    0.408
_exptl_absorpt_correction_T_max  0.918
_exptl_absorpt_correction_T_min  0.829
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_density_diffrn    1.273
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.489
_refine_diff_density_min         -0.633
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    'riding; torsion refined for o-methyls'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     621
_refine_ls_number_reflns         11383
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0897
_refine_ls_R_factor_gt           0.0516
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0373P)^2^+1.7152P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1054
_refine_ls_wR_factor_ref         0.1189
_reflns_number_gt                7910
_reflns_number_total             11383
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b210467a.txt
_cod_data_source_block           may1302
_cod_original_cell_volume        2517.63(8)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7012377