Selective crystallization of four bis(phthalocyaninato)lanthanoid(iii) polymorphs
Dailey, Maegan; Besson, Claire; CrystEngComm 23 (2021) 7151–7161; doi:10.1039/D1CE00936B

data_7243607
_publ_section_title
;
 Selective crystallization of four bis(phthalocyaninato)lanthanoid(iii)
 polymorphs
;
_journal_issue                   40
_journal_name_full               CrystEngComm
_journal_page_first              7151
_journal_page_last               7161
_journal_paper_doi               10.1039/D1CE00936B
_journal_volume                  23
_journal_year                    2021
_chemical_formula_moiety         'C64 H32 N16 Pr, C Cl2 H2'
_chemical_formula_sum            'C65 H34 Cl2 N16 Pr'
_chemical_formula_weight         1250.89
_chemical_name_common            bis(phthalocyaninato)-praseodymium
_chemical_name_systematic
(phthalocyaninato)-(phthalocyaninato-radical)-praseodymium(III)
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-09-09 deposited with the CCDC.	2021-09-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   28.1128(16)
_cell_length_b                   22.9663(14)
_cell_length_c                   7.8883(5)
_cell_measurement_reflns_used    165689
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      60.961
_cell_measurement_theta_min      5.364
_cell_volume                     5093.1(5)
_computing_cell_refinement       'APEX3 v2019.1-0 (Bruker AXS)'
_computing_data_collection       'Bruker Instrument Service V6.2.132'
_computing_data_reduction        'SAINT V8.40A (Bruker Nano Inc., 2019)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle rev 958)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0972
_diffrn_reflns_av_unetI/netI     0.0294
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            157510
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.515
_diffrn_reflns_theta_min         2.290
_diffrn_source                   'microfocus sealed tube'
_exptl_absorpt_coefficient_mu    1.126
_exptl_absorpt_correction_T_max  0.7421
_exptl_absorpt_correction_T_min  0.7002
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2016/2 (G. Sheldrick)'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.631
_exptl_crystal_description       needle
_exptl_crystal_F_000             2516
_exptl_crystal_recrystallization_method 'slow evaporation from DCM'
_exptl_crystal_size_max          4.628
_exptl_crystal_size_mid          0.219
_exptl_crystal_size_min          0.068
_refine_diff_density_max         0.995
_refine_diff_density_min         -0.765
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         7956
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0385
_refine_ls_R_factor_gt           0.0294
_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^)+(0.0282P)^2^+8.1475P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0708
_refine_ls_wR_factor_ref         0.0752
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6883
_reflns_number_total             7956
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce00936b2.cif
_cod_data_source_block           PrPc2_Pnma
_cod_depositor_comments
'Adding full bibliography for 7243585--7243607.cif.'
_cod_database_code               7243607
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              88394