Synthesis and reactivity of aza-dipyrrin alkali metal salts.
Diaz-Rodriguez, Roberto M; Robertson, Katherine N.; Thompson, Alison; Chemical communications (Cambridge, England) 54 (2018) 13139–13142; doi:10.1039/c8cc07101b

data_7122558
_publ_section_title
;
 Synthesis and reactivity of aza-dipyrrin alkali metal salts.
;
_journal_issue                   93
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              13139
_journal_page_last               13142
_journal_paper_doi               10.1039/c8cc07101b
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         'C36 H30 Cl N3 O Zn'
_chemical_formula_sum            'C36 H30 Cl N3 O Zn'
_chemical_formula_weight         621.45
_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-2018/1
_audit_update_record
;
2018-08-22 deposited with the CCDC.
2018-10-26 downloaded from the CCDC.
;
_cell_angle_alpha                103.459(2)
_cell_angle_beta                 92.281(2)
_cell_angle_gamma                97.662(2)
_cell_formula_units_Z            4
_cell_length_a                   8.3304(13)
_cell_length_b                   13.730(2)
_cell_length_c                   26.735(4)
_cell_measurement_reflns_used    6704
_cell_measurement_temperature    125(2)
_cell_measurement_theta_max      27.25
_cell_measurement_theta_min      2.36
_cell_volume                     2939.4(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      125(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.909
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0935
_diffrn_reflns_av_unetI/netI     0.1497
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.909
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            34672
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.909
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.773
_diffrn_reflns_theta_min         1.542
_exptl_absorpt_coefficient_mu    0.961
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6336
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Bruker 2009'
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.404
_exptl_crystal_description       'very thin rectangular needles'
_exptl_crystal_F_000             1288
_exptl_crystal_size_max          0.750
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.025
_refine_diff_density_max         0.647
_refine_diff_density_min         -0.707
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.970
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     757
_refine_ls_number_reflns         13926
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.970
_refine_ls_R_factor_all          0.1428
_refine_ls_R_factor_gt           0.0589
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'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          0.0950
_refine_ls_wR_factor_ref         0.1182
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7336
_reflns_number_total             13926
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc07101b2.cif
_cod_data_source_block           RD009B_LT_3a
_cod_depositor_comments
'Adding full bibliography for 7122556--7122558.cif.'
_cod_original_cell_volume        2939.5(8)
_cod_database_code               7122558
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_min   0.533
_shelx_estimated_absorpt_t_max   0.976
_shelx_res_checksum              92944
_shelx_hkl_checksum              33603