Tautomerisation and hydrogen-bonding interactions in four-coordinate metal halide and azide complexes of N-donor-extended dipyrromethanes.
Reid, Stuart D.; Wilson, Claire; Blake, Alexander J.; Love, Jason B.; Dalton transactions (Cambridge, England : 2003) 39 (2010) 418–425; doi:10.1039/b909842a

data_7024062
_publ_section_title
;
 Tautomerisation and hydrogen-bonding interactions in four-coordinate
 metal halide and azide complexes of N-donor-extended dipyrromethanes.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              418
_journal_page_last               425
_journal_paper_doi               10.1039/b909842a
_journal_volume                  39
_journal_year                    2010
_chemical_formula_moiety         'C21 H32 Br2 Fe N4'
_chemical_formula_sum            'C21 H32 Br2 Fe N4'
_chemical_formula_weight         556.16
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     'Patterson heavy-atom'
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                99.138(2)
_cell_angle_beta                 96.256(2)
_cell_angle_gamma                92.283(2)
_cell_formula_units_Z            2
_cell_length_a                   8.9170(8)
_cell_length_b                   9.4120(9)
_cell_length_c                   14.4922(14)
_cell_measurement_reflns_used    3844
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.4
_cell_volume                     1191.67(19)
_computing_cell_refinement       'Bruker SAINT version 6.36a (Bruker, 2000)'
_computing_data_collection       'Bruker SMART version 5.625 (Bruker, 2001)'
_computing_data_reduction        'Bruker SAINT; Bruker SHELXTL (Bruker, 2001)'
_computing_publication_material  'enCIFer (CCDC, 2003); PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.943
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       omega
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.024
_diffrn_reflns_av_sigmaI/netI    0.032
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            7254
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         2.42
_diffrn_source                   'normal-focus sealed tube'
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    3.999
_exptl_absorpt_correction_T_max  0.122
_exptl_absorpt_correction_T_min  0.0610
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SHELXTL version 6.12; Bruker, 2001)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.550
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tablet
_exptl_crystal_F_000             564
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.58
_refine_diff_density_min         -0.26
_refine_diff_density_rms         0.07
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.94
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         5169
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.94
_refine_ls_R_factor_all          0.0340
_refine_ls_R_factor_gt           0.0267
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0364P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0619
_refine_ls_wR_factor_ref         0.0631
_reflns_number_gt                4257
_reflns_number_total             5172
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b909842a.txt
_cod_data_source_block           FE2MTB
_cod_original_cell_volume        1191.7(3)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7024062