Self-assembly of bis-β-diketone-based [M2L2] dinuclear platforms into 2-dimensional coordination polymers
Brock, A. J.; McMurtrie, John C.; Clegg, J. K.; CrystEngComm 21 (2019) 4786–; doi:10.1039/C9CE00896A

data_7233134
_publ_section_title
;
 Self-assembly of bis-\b-diketone-based [M2L2] dinuclear platforms into
 2-dimensional coordination polymers
;
_journal_issue                   32
_journal_name_full               CrystEngComm
_journal_page_first              4786
_journal_paper_doi               10.1039/C9CE00896A
_journal_volume                  21
_journal_year                    2019
_chemical_formula_moiety         'C38 H46 N2 O8 Pd2'
_chemical_formula_sum            'C38 H46 N2 O8 Pd2'
_chemical_formula_weight         871.57
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-05-09
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-05-09 deposited with the CCDC.    2019-07-12 downloaded from the CCDC.
;
_cell_angle_alpha                75.20(3)
_cell_angle_beta                 88.40(3)
_cell_angle_gamma                74.52(3)
_cell_formula_units_Z            1
_cell_length_a                   5.7610(12)
_cell_length_b                   9.921(2)
_cell_length_c                   16.902(3)
_cell_measurement_reflns_used    3298
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.373
_cell_measurement_theta_min      2.205
_cell_volume                     899.3(4)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.898
_diffrn_measured_fraction_theta_max 0.895
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'Phi Scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7108
_diffrn_reflns_av_unetI/netI     0.0316
_diffrn_reflns_Laue_measured_fraction_full 0.898
_diffrn_reflns_Laue_measured_fraction_max 0.895
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            3298
_diffrn_reflns_point_group_measured_fraction_full 0.898
_diffrn_reflns_point_group_measured_fraction_max 0.895
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.373
_diffrn_reflns_theta_min         2.205
_exptl_absorpt_coefficient_mu    1.055
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.609
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             444
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         3.895
_refine_diff_density_min         -3.610
_refine_diff_density_rms         0.415
_refine_ls_extinction_coef       0.084(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.224
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         3298
_refine_ls_number_restraints     209
_refine_ls_restrained_S_all      1.185
_refine_ls_R_factor_all          0.1365
_refine_ls_R_factor_gt           0.1360
_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^)+(0.0159P)^2^+62.3045P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3838
_refine_ls_wR_factor_ref         0.3839
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3253
_reflns_number_total             3298
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce00896a2.cif
_cod_data_source_block           p1_a
_cod_depositor_comments
'Adding full bibliography for 7233133--7233136.cif.'
_cod_original_cell_volume        899.2(4)
_cod_database_code               7233134
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.603(8)
 0.397(8)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(C10A)=Sof(H10D)=Sof(H10E)=Sof(H10F)=Sof(C15A)=Sof(H15D)=Sof(H15E)=
 Sof(H15F)=Sof(C12A)=Sof(H12D)=Sof(H12E)=Sof(H12F)=1-FVAR(1)
 Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(H10C)=Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(H12C)=
 Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(H15C)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C14(H14), C6(H6), C9(H9), C9AA(H9AA), C3AA(H3AA)
5.b Fitted hexagon refined as free rotating group:
 C9(C2AA,C9AA,N1,C3AA,C8)
5.c Idealised Me refined as rotating group:
 C0CA(H0CA,H0CB,H0CC), C1AA(H1AA,H1AB,H1AC), C0AA(H0AA,H0AB,H0AC), C10(H10A,
 H10B,H10C), C12(H12A,H12B,H12C), C15(H15A,H15B,H15C), C10A(H10D,H10E,H10F),
 C15A(H15D,H15E,H15F), C12A(H12D,H12E,H12F)
;
_shelx_res_checksum              43874
_olex2_submission_special_instructions 'No special instructions were received'