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

data_7243592
_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         1187.55
_chemical_name_common            bis(phthalocyaninato)-dysprosium
_chemical_name_systematic
(phthalocyaninato)-(phthalocyaninato-radical)-dysprosium(III)
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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                   8.8171(11)
_cell_length_b                   10.5671(12)
_cell_length_c                   50.648(6)
_cell_measurement_reflns_used    42761
_cell_measurement_temperature    102(2)
_cell_measurement_theta_max      58.983
_cell_measurement_theta_min      4.547
_cell_volume                     4718.9(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      102(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.980
_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  0.0506
_diffrn_reflns_av_unetI/netI     0.0684
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       59
_diffrn_reflns_limit_l_min       -72
_diffrn_reflns_number            42659
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.496
_diffrn_reflns_theta_min         1.969
_diffrn_source                   'fine-focused sealed tube'
_exptl_absorpt_coefficient_mu    1.650
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6232
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2016/2 (G. Sheldrick)'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.672
_exptl_crystal_description       block
_exptl_crystal_F_000             2376
_exptl_crystal_recrystallization_method 'slow evaporation from CHCl3'
_exptl_crystal_size_max          3.764
_exptl_crystal_size_mid          0.275
_exptl_crystal_size_min          0.189
_refine_diff_density_max         1.238
_refine_diff_density_min         -2.652
_refine_diff_density_rms         0.123
_refine_ls_abs_structure_details
;
 Flack x determined using 4623 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.011(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     730
_refine_ls_number_reflns         13851
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.0535
_refine_ls_R_factor_gt           0.0457
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0215P)^2^+3.8056P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0812
_refine_ls_wR_factor_ref         0.0833
_reflns_Friedel_coverage         0.758
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.939
_reflns_number_gt                12585
_reflns_number_total             13851
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce00936b2.cif
_cod_data_source_block           DyPc2_P212121
_cod_depositor_comments
'Adding full bibliography for 7243585--7243607.cif.'
_cod_original_cell_volume        4719.0(9)
_cod_database_code               7243592
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.063
_shelx_estimated_absorpt_t_max   0.746
_shelx_res_checksum              13146