Control over coordination self-assembly of flexible, multidentate ligands by stepwise metal coordination of isopyrazole subunits.
Ashida, Yoshiko; Manabe, Yumehiro; Yoshioka, Shota; Yoneda, Tomoki; Inokuma, Yasuhide; Dalton transactions (Cambridge, England : 2003) 48 (2019) 818–822; doi:10.1039/c8dt04935a

data_7048381
_publ_section_title
;
 Control over coordination self-assembly of flexible, multidentate ligands
 by stepwise metal coordination of isopyrazole subunits.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              818
_journal_page_last               822
_journal_paper_doi               10.1039/c8dt04935a
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C56 H84 N16 Pd2, 4(BF4), 2.574(H2O)'
_chemical_formula_sum            'C56 H89.15 B4 F16 N16 O2.57 Pd2'
_chemical_formula_weight         1587.79
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2018-12-15 deposited with the CCDC.
2018-12-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.940(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.9729(3)
_cell_length_b                   14.3355(3)
_cell_length_c                   37.3886(7)
_cell_measurement_reflns_used    41119
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      29.6520
_cell_measurement_theta_min      2.6470
_cell_volume                     6949.3(3)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.852
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RCD3): quarter-chi single'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0388
_diffrn_reflns_av_unetI/netI     0.0323
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.852
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            72930
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.852
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.541
_diffrn_reflns_theta_min         2.406
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'XtaLAB AFC11 (RCD3): quarter-chi single'
_exptl_absorpt_coefficient_mu    0.614
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72874
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.43a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.518
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3255
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.070
_refine_diff_density_max         1.023
_refine_diff_density_min         -1.028
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1023
_refine_ls_number_reflns         16533
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.131
_refine_ls_R_factor_all          0.0576
_refine_ls_R_factor_gt           0.0472
_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^)+(0.0220P)^2^+16.7719P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0940
_refine_ls_wR_factor_ref         0.0971
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14071
_reflns_number_total             16533
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04935a2.cif
_cod_data_source_block           Pd2L2
_cod_depositor_comments
'Adding full bibliography for 7048378--7048381.cif.'
_cod_database_code               7048381
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.852
_shelx_estimated_absorpt_t_max   0.958
_shelx_res_checksum              89964