Side-on Bound Complexes of Phenyl- and Methyl-diazene
Leslie D. Field; Hsiu L. Li; Scott J. Dalgarno; Ruaraidh D. McIntosh; Inorganic Chemistry 51 (2012) 3733–3742; doi:10.1021/ic2027225

data_4328683
_publ_section_title
;
 Side-on Bound Complexes of Phenyl- and Methyl-diazene
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3733
_journal_page_last               3742
_journal_paper_doi               10.1021/ic2027225
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C22 H47 Cl Fe N2 O P4'
_chemical_formula_weight         570.80
_chemical_name_common            LHL2284
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 106.257(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.260(2)
_cell_length_b                   13.4299(16)
_cell_length_c                   12.5230(14)
_cell_measurement_reflns_used    925
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.88
_cell_measurement_theta_min      2.35
_cell_volume                     2786.8(6)
_computing_cell_refinement       'SAINT (Bruker, 1998)'
_computing_data_collection       'Apex II'
_computing_data_reduction        'SAINT (Bruker, 1998)'
_computing_molecular_graphics    'XSeed (Barbour, 2001)'
_computing_publication_material  'local program'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'Bruker Nonius X8 Apex II CCD Diffractometer'
_diffrn_measurement_method       '\f and \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  0.0464
_diffrn_reflns_av_sigmaI/netI    0.1517
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7171
_diffrn_reflns_theta_full        29.03
_diffrn_reflns_theta_max         29.03
_diffrn_reflns_theta_min         2.35
_exptl_absorpt_coefficient_mu    0.884
_exptl_absorpt_correction_T_max  0.9326
_exptl_absorpt_correction_T_min  0.8158
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Bruker-SADABS
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.360
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1216
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.516
_refine_diff_density_min         -0.783
_refine_diff_density_rms         0.156
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         7173
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.1531
_refine_ls_R_factor_gt           0.0714
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0319P)^2^+5.0561P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1100
_refine_ls_wR_factor_ref         0.1344
_reflns_number_gt                4115
_reflns_number_total             7173
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2027225_si_001_1.cif
_cod_data_source_block           LHL2284
_cod_original_cell_volume        2786.7(6)
_cod_database_code               4328683