A Rare μ-Hydroxo-Bridged Species. Synthesis, Structure, and Properties of μ-Hydroxo(tetraphenylporphyrinatomanganese(III))(phthalocyaninato(azido)chromium(III)), [(TPP)Mn−O(H)−CrPc(N3)]
Donzello, Maria Pia; Bartolino, Laura; Ercolani, Claudio; Rizzoli, Corrado; Inorganic Chemistry 45 (2006) 6988–6995; doi:10.1021/ic060574q

data_4332625
_publ_section_title
;
 A Rare \m-Hydroxo-Bridged Species. Synthesis, Structure, and Properties
 of
 \m-Hydroxo(tetraphenylporphyrinatomanganese(III))(phthalocyaninato(azido)chromium(III)),
 [(TPP)Mn&#x2212;O(H)&#x2212;CrPc(N3)]
;
_journal_issue                   17
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6988
_journal_page_last               6995
_journal_paper_doi               10.1021/ic060574q
_journal_volume                  45
_journal_year                    2006
_chemical_formula_moiety         'C76 H45 Cr Mn N15 O1, 2(C10 H7 Cl)'
_chemical_formula_sum            'C96 H59 Cl2 Cr Mn N15 O'
_chemical_formula_weight         1616.43
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 98.79(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4.00
_cell_length_a                   16.645(3)
_cell_length_b                   17.692(4)
_cell_length_c                   25.828(5)
_cell_measurement_reflns_used    712
_cell_measurement_temperature    143
_cell_measurement_theta_max      23.3
_cell_measurement_theta_min      12.4
_cell_volume                     7517(3)
_computing_cell_refinement
'marHKL (release 1.9.1), based on HKL (Otwinowski & Minor, 1997)'
_computing_data_collection       'MAR345 Software (MARresearch, 1999)'
_computing_data_reduction        marHKL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      143(2)
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.99
_diffrn_measurement_device       'MAR345 IPDS'
_diffrn_measurement_method       '\f scan (\D\f = 3\%; exp. time 180 s)'
_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  0.0696
_diffrn_reflns_av_sigmaI/netI    0.0850
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            32300
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         24.85
_diffrn_reflns_theta_min         1.95
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.4483
_exptl_absorpt_correction_T_max  0.971
_exptl_absorpt_correction_T_min  0.951
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.4284
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    not_measured
_exptl_crystal_description       'irregular prism'
_exptl_crystal_F_000             3324.0
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.875
_refine_diff_density_min         -1.024
_refine_diff_density_rms         0.100
_refine_ls_extinction_coef       0.0016(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1002
_refine_ls_number_reflns         10470
_refine_ls_number_restraints     192
_refine_ls_restrained_S_all      1.161
_refine_ls_R_factor_all          0.1333
_refine_ls_R_factor_gt           0.0860
_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^)+(0.1685P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2433
_refine_ls_wR_factor_ref         0.2671
_reflns_number_gt                6394
_reflns_number_total             12627
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic060574qsup1.cif
_cod_data_source_block           '[Mn-Cr]'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not_measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C96 H59 Cl2 Cr1 Mn1 N15 O1'
_cod_database_code               4332625