Deprotonated meso-hydroxyporphyrin as a stable π-electronic anion: the building unit of ion-pairing assembly
Sasano, Yoshifumi; Yasuda, Nobuhiro; Maeda, Hiromitsu; Dalton Trans.  (2017) –; doi:10.1039/C7DT01635B

data_7042957
_publ_section_title
;
 Deprotonated meso-hydroxyporphyrin as a stable \p-electronic anion: the
 building unit of ion-pairing assembly
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT01635B
_journal_year                    2017
_chemical_formula_sum            'C44 H21.5 F15 N4 Ni O3'
_chemical_formula_weight         997.86
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2017-03-07 deposited with the CCDC.
2017-05-10 downloaded from the CCDC.
;
_cell_angle_alpha                72.365(5)
_cell_angle_beta                 80.781(6)
_cell_angle_gamma                78.319(6)
_cell_formula_units_Z            2
_cell_length_a                   7.309(3)
_cell_length_b                   14.459(6)
_cell_length_c                   20.126(8)
_cell_measurement_reflns_used    19562
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.060
_cell_measurement_theta_min      1.052
_cell_volume                     1973.8(14)
_computing_cell_refinement       RAPID-AUTO
_computing_data_collection       RAPID-AUTO
_computing_data_reduction        RAPID-AUTO
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Rigaku MercuryCCD2'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'Si 311'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7006
_diffrn_reflns_av_R_equivalents  0.1536
_diffrn_reflns_av_unetI/netI     0.2367
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            19562
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        24.857
_diffrn_reflns_theta_max         27.060
_diffrn_reflns_theta_min         1.052
_exptl_absorpt_coefficient_mu    0.586
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.679
_exptl_crystal_description       needle
_exptl_crystal_F_000             1001
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.568
_refine_diff_density_min         -1.112
_refine_diff_density_rms         0.197
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     616
_refine_ls_number_reflns         8927
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.2688
_refine_ls_R_factor_gt           0.1424
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.2000P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3412
_refine_ls_wR_factor_ref         0.4202
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3605
_reflns_number_total             8927
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01635b2.cif
_cod_data_source_block           shelx
_cod_original_cell_volume        1974.0(14)
_cod_original_formula_sum        'C44 H21.50 F15 N4 Ni O3'
_cod_database_code               7042957
_shelx_estimated_absorpt_t_min   0.944
_shelx_estimated_absorpt_t_max   0.944
_shelxl_version_number           2013-2
_shelx_res_checksum              85826