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

data_7243606
_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 Nd'
_chemical_formula_sum            'C64 H32 N16 Nd'
_chemical_formula_weight         1169.29
_chemical_name_common            '(bis)phthalocyanine neodymium'
_chemical_name_systematic
'[phthalocyaninato]-[phthalocyaninato-radical]neodymium(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
;
2021-07-17 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                   8.852(2)
_cell_length_b                   10.604(2)
_cell_length_c                   50.844(12)
_cell_measurement_reflns_used    11392
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.0
_cell_measurement_theta_min      0.8
_cell_volume                     4772.6(18)
_computing_cell_refinement       'SAINT V8.37A, Bruker-AXS'
_computing_data_collection       'APEX, Bruker-AXS'
_computing_data_reduction        'SAINT V8.37A, Bruker-AXS'
_computing_molecular_graphics    'WinGX (Farrugia, 2012)'
_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 0.993
_diffrn_measurement_device_type  'Bruker Smart APEX II'
_diffrn_measurement_method       'Omega scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0613
_diffrn_reflns_av_unetI/netI     0.0469
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       64
_diffrn_reflns_limit_l_min       -66
_diffrn_reflns_number            69514
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         28.009
_diffrn_reflns_theta_min         2.266
_diffrn_source                   'fine-focused sealed tube'
_diffrn_source_type              'Bruker Smart APEX II'
_exptl_absorpt_coefficient_mu    1.154
_exptl_absorpt_correction_T_max  0.9744
_exptl_absorpt_correction_T_min  0.8905
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2014/5. G. Sheldrick'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.627
_exptl_crystal_description       block
_exptl_crystal_F_000             2352
_exptl_crystal_recrystallization_method 'slow evaporation from chloroform'
_exptl_transmission_factor_max   0.95071
_exptl_transmission_factor_min   0.91311
_refine_diff_density_max         0.777
_refine_diff_density_min         -0.918
_refine_diff_density_rms         0.082
_refine_ls_abs_structure_details
;
 Flack x determined using 4338 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.004(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.859
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     730
_refine_ls_number_reflns         11389
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.859
_refine_ls_R_factor_all          0.0345
_refine_ls_R_factor_gt           0.0307
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0515P)^2^+3.1914P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0720
_refine_ls_wR_factor_ref         0.0739
_reflns_Friedel_coverage         0.768
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.980
_reflns_number_gt                10691
_reflns_number_total             11389
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce00936b2.cif
_cod_data_source_block           NdPc2_P212121
_cod_depositor_comments
'Adding full bibliography for 7243585--7243607.cif.'
_cod_original_cell_volume        4772.5(19)
_cod_database_code               7243606
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              23177