Infinite Coordination Polymer Particles Composed of Stimuli-Responsive Coordination Complex Subunits
d’Aquino, Andrea I.; Kean, Zachary S.; Mirkin, Chad A.; Chemistry of Materials 29 (2017) 10284–; doi:10.1021/acs.chemmater.7b03638

data_4002880
_publ_section_title
;
 Infinite Coordination Polymer Particles Composed of Stimuli-Responsive
 Coordination Complex Subunits
;
_journal_issue                   24
_journal_name_full               'Chemistry of Materials'
_journal_page_first              10284
_journal_paper_doi               10.1021/acs.chemmater.7b03638
_journal_volume                  29
_journal_year                    2017
_chemical_formula_moiety         'C72 H60 N6 P2 Pd S2, C4 H10 O, 2(B F4)'
_chemical_formula_sum            'C76 H70 B2 F8 N6 O P2 Pd S2'
_chemical_formula_weight         1489.46
_chemical_name_systematic
;
 ?
;
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-06-06
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 92.515(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.5073(5)
_cell_length_b                   35.1644(18)
_cell_length_c                   21.6818(11)
_cell_measurement_reflns_used    9893
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      68.076
_cell_measurement_theta_min      4.271
_cell_volume                     7241.6(6)
_computing_cell_refinement       'SAINT V8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 V2014.11-0 (Bruker, 2014)'
_computing_data_reduction        'Bruker SAINT'
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      149.99
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Bruker Kappa APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'MX optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0642
_diffrn_reflns_av_unetI/netI     0.0719
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            34154
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.317
_diffrn_reflns_theta_min         2.513
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    3.601
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.5720
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0934 before and 0.0593 after correction.
The Ratio of minimum to maximum transmission is 0.7595.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.366
_exptl_crystal_description       plate
_exptl_crystal_F_000             3064
_exptl_crystal_size_max          0.259
_exptl_crystal_size_mid          0.095
_exptl_crystal_size_min          0.006
_refine_diff_density_max         0.939
_refine_diff_density_min         -0.938
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1033
_refine_ls_number_reflns         12892
_refine_ls_number_restraints     534
_refine_ls_restrained_S_all      1.139
_refine_ls_R_factor_all          0.0803
_refine_ls_R_factor_gt           0.0605
_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^)+(0.0858P)^2^+5.0173P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1515
_refine_ls_wR_factor_ref         0.1607
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9935
_reflns_number_total             12892
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm7b03638_si_002.cif
_cod_data_source_block           cx0777
_cod_depositor_comments          'Adding full bibliography for 4002880.cif.'
_cod_database_code               4002880
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.979
_shelx_estimated_absorpt_t_min   0.456
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C18-C17 \\sim C21A-C20A \\sim C17-C16 \\sim C21A-C16 \\sim C17A-C16 \\sim
C21-C16 \\sim C21-C20 ~
 C18A-C17A \\sim C20-C19 \\sim C19-C18A \\sim C20A-C19 \\sim C19-C18
 with sigma of 0.01
 C64-C63 \\sim C64A-C63A \\sim C65-C64 \\sim C65A-C64A \\sim C66-C65 \\sim
C66A-C65A \\sim C67-C66 ~
 C67A-C66A
 with sigma of 0.01
 N5-C63 \\sim N5A-C63A \\sim N5-C67 \\sim N5A-C67A
 with sigma of 0.01
 C63-C61 \\sim C63A-C61
 with sigma of 0.01
 F5A-B2 \\sim F8-B2 \\sim F8A-B2 \\sim F6A-B2 \\sim F6-B2 \\sim F5-B2 \\sim
F7-B2
 with sigma of 0.005
3. Rigid bond restraints
 C17, C17A, C18, C18A, C20, C20A, C21, C21A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C28, C28A, C29, C29A, C30, C30A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N5, N5A, C63, C63A, C64, C64A, C65, C65A, C66, C66A, C67, C67A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 F5, F5A, F6, F6A, F8, F8A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C17 \\sim C17A \\sim C18 \\sim C18A \\sim C20 \\sim C20A \\sim C21 \\sim C21A:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C28 \\sim C28A \\sim C29 \\sim C29A \\sim C30 \\sim C30A: within 2A with sigma
of 0.04 and sigma for terminal atoms of 0.08
N5 \\sim N5A \\sim C63 \\sim C63A \\sim C64 \\sim C64A \\sim C65 \\sim C65A
\\sim C66 \\sim C66A \\sim C67 \\sim C67A: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
F5 \\sim F5A \\sim F6 \\sim F6A \\sim F8 \\sim F8A: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08
5. Others
 Sof(C17A)=Sof(H17A)=Sof(C18A)=Sof(H18A)=Sof(C20A)=Sof(H20A)=Sof(C21A)=
 Sof(H21A)=1-FVAR(1)
 Sof(C17)=Sof(H17)=Sof(C18)=Sof(H18)=Sof(C20)=Sof(H20)=Sof(C21)=Sof(H21)=FVAR(1)
 Sof(C28A)=Sof(H28A)=Sof(C29A)=Sof(H29A)=Sof(C30A)=Sof(H30A)=Sof(H31A)=1-FVAR(2)
 Sof(C28)=Sof(H28)=Sof(C29)=Sof(H29)=Sof(C30)=Sof(H30)=Sof(H31)=FVAR(2)
 Sof(N5A)=Sof(C63A)=Sof(C64A)=Sof(H64A)=Sof(C65A)=Sof(H65A)=Sof(C66A)=
 Sof(H66A)=Sof(C67A)=Sof(H67A)=1-FVAR(3)
 Sof(C63)=Sof(C64)=Sof(H64)=Sof(C65)=Sof(H65)=Sof(C66)=Sof(H66)=Sof(C67)=
 Sof(H67)=Sof(N5)=FVAR(3)
 Sof(F5A)=Sof(F6A)=Sof(F8A)=1-FVAR(4)
 Sof(F5)=Sof(F6)=Sof(F8)=FVAR(4)
6.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C49(H49A,H49B), C50(H50A,
 H50B), C51(H51A,H51B), C74(H74A,H74B), C75(H75A,H75B)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C17(H17), C17A(H17A), C18(H18), C18A(H18A), C20(H20), C20A(H20A),
 C21(H21), C21A(H21A), C23(H23), C26(H26), C28(H28), C28A(H28A), C29(H29),
 C29A(H29A), C30(H30), C30A(H30A), C31(H31), C31(H31A), C33(H33), C34(H34),
 C35(H35), C36(H36), C38(H38), C39(H39), C40(H40), C41(H41), C42(H42), C44(H44),
  C45(H45), C46(H46), C47(H47), C48(H48), C53(H53), C54(H54), C56(H56),
 C57(H57), C59(H59), C62(H62), C64(H64), C65(H65), C66(H66), C67(H67),
 C64A(H64A), C65A(H65A), C66A(H66A), C67A(H67A), C72(H72), C71(H71), C70(H70),
 C69(H69)
6.c Idealised Me refined as rotating group:
 C73(H73A,H73B,H73C), C76(H76A,H76B,H76C)
;
_smtbx_masks_special_details
;
The solvent masking procedure as implemented in Olex2 was used to remove the
electronic contribution of solvent molecules from the refinement.  As the exact
solvent content is not known, only the atoms used in the refinement model are
reported in the formula here.

Total solvent accessible volume / cell = 426.5 Ang^3^ [5.9%]
Total electron count / cell = 73.8
;
_shelx_res_checksum              87431
_shelx_hkl_checksum              70819
_olex2_date_sample_data_collection 2016-06-03
_olex2_date_sample_submission    2016-05-31
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a glass fibre in Paratone oil'
_olex2_submission_original_sample_id cx0777
_olex2_submission_special_instructions 'No special instructions were received'