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_7048380
_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
'C42 H66 N12 Pd2, 4(B F4), 2.616(C H2 Cl2), 0.692(O)'
_chemical_formula_sum            'C22.31 H35.62 B2 Cl2.31 F8 N6 O0.35 Pd'
_chemical_formula_weight         755.27
_space_group_crystal_system      orthorhombic
_space_group_IT_number           40
_space_group_name_Hall           'A 2 -2a'
_space_group_name_H-M_alt        'A m a 2'
_symmetry_space_group_name_Hall  'A 2 -2a'
_symmetry_space_group_name_H-M   'A m a 2'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2018-12-15 deposited with the CCDC.
2018-12-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.6757(6)
_cell_length_b                   21.3064(6)
_cell_length_c                   11.7797(3)
_cell_measurement_reflns_used    27530
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      1.91
_cell_volume                     6444.2(3)
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector                 'Image Plate'
_diffrn_detector_area_resol_mean 10
_diffrn_detector_type            'Rigaku IP'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  RAPID
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0424
_diffrn_reflns_av_unetI/netI     0.0361
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            30719
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.481
_diffrn_reflns_theta_min         1.912
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.839
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6647
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR(Rigaku, 1995)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.557
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3052
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.155
_refine_diff_density_min         -0.987
_refine_diff_density_rms         0.121
_refine_ls_abs_structure_details
;
 Flack x determined using 2925 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.041(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     429
_refine_ls_number_reflns         7515
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.0604
_refine_ls_R_factor_gt           0.0561
_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^)+(0.0826P)^2^+17.2054P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1401
_refine_ls_wR_factor_ref         0.1423
_reflns_Friedel_coverage         0.896
_reflns_Friedel_fraction_full    0.992
_reflns_Friedel_fraction_max     0.987
_reflns_number_gt                7069
_reflns_number_total             7515
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04935a2.cif
_cod_data_source_block           Pd2L3
_cod_depositor_comments
'Adding full bibliography for 7048378--7048381.cif.'
_cod_database_code               7048380
_shelx_shelxl_version_number     2017/1
_shelx_res_checksum              7968