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

data_7243597
_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 Dy N16'
_chemical_formula_sum            'C64 H32 Dy N16'
_chemical_formula_weight         1187.54
_chemical_name_common            'bis(phthalocyaninato) dysprosium'
_chemical_name_systematic
(phthalocyaninato)-(phthalocyaninato-radical)-dysprosium(III)
_space_group_crystal_system      tetragonal
_space_group_IT_number           126
_space_group_name_Hall           '-P 4a 2bc'
_space_group_name_H-M_alt        'P 4/n n c :2'
_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                90.00(3)
_cell_angle_beta                 90.00(3)
_cell_angle_gamma                90.00(3)
_cell_formula_units_Z            2
_cell_length_a                   19.548(4)
_cell_length_b                   19.548(4)
_cell_length_c                   6.477(2)
_cell_measurement_reflns_used    8287
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      55.401
_cell_measurement_theta_min      6.585
_cell_volume                     2475.0(10)
_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      293(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       '\f and \w scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1173
_diffrn_reflns_av_unetI/netI     0.0155
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            1493
_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         27.897
_diffrn_reflns_theta_min         2.084
_diffrn_source                   'micro-focused sealed tube'
_exptl_absorpt_coefficient_mu    1.573
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2016/2 (G. Sheldrick)'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.584
_exptl_crystal_description       rectangle
_exptl_crystal_F_000             1183
_exptl_crystal_recrystallization_method 'slow evaporation from CHCl3:EtOH'
_exptl_crystal_size_max          1.175
_exptl_crystal_size_mid          0.131
_exptl_crystal_size_min          0.050
_exptl_transmission_factor_max   0.745618
_exptl_transmission_factor_min   0.619239
_refine_diff_density_max         3.398
_refine_diff_density_min         -0.858
_refine_diff_density_rms         0.180
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.509
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     94
_refine_ls_number_reflns         1493
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.509
_refine_ls_R_factor_all          0.0702
_refine_ls_R_factor_gt           0.0700
_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^)+(0.0659P)^2^+16.2423P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1907
_refine_ls_wR_factor_ref         0.1909
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1488
_reflns_number_total             1493
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce00936b2.cif
_cod_data_source_block           DyPc2_P4nnc
_cod_depositor_comments
'Adding full bibliography for 7243585--7243607.cif.'
_cod_original_cell_volume        2475.2(13)
_cod_original_sg_symbol_H-M      'P 4/n n c'
_cod_database_code               7243597
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              49491