Controlling orthogonal self-assembly through cis-trans isomerization of a non-covalent palladium complex dimer.
Kokan, Zoran; Kovačević, Borislav; Štefanić, Zoran; Tzvetkova, Pavleta; Kirin, Srećko I; Chemical communications (Cambridge, England) 54 (2018) 2094–2097; doi:10.1039/c7cc09537f

data_7121056
_publ_section_title
;
 Controlling orthogonal self-assembly through cis-trans isomerization of a
 non-covalent palladium complex dimer.
;
_journal_issue                   17
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              2094
_journal_page_last               2097
_journal_paper_doi               10.1039/c7cc09537f
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         'C52 H54 Cl2 N8 O8 P2 Pd'
_chemical_formula_sum            'C52 H54 Cl2 N8 O8 P2 Pd'
_chemical_formula_weight         1158.27
_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'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-07-24
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2017-07-24 deposited with the CCDC.
2018-01-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.7533(11)
_cell_length_b                   21.7745(11)
_cell_length_c                   29.714(2)
_cell_measurement_reflns_used    5290
_cell_measurement_temperature    99.98(19)
_cell_measurement_theta_max      52.0360
_cell_measurement_theta_min      4.3070
_cell_volume                     12133.5(12)
_computing_cell_refinement       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.98(19)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.947
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -17.00  50.00   0.50  115.00    --   52.92 -37.00   0.00  134
  2  \w     59.00  96.00   0.50  115.00    --   52.92-125.00  60.00   74
  3  \w   -121.00 -82.00   0.50  115.00    --  -54.48-125.00 -60.00   78
  4  \w   -125.00 -36.00   0.50  115.00    --  -54.48 -77.00   0.00  178
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0718251000
_diffrn_orient_matrix_UB_12      -0.0304216000
_diffrn_orient_matrix_UB_13      -0.0117123000
_diffrn_orient_matrix_UB_21      -0.0343808000
_diffrn_orient_matrix_UB_22      -0.0639565000
_diffrn_orient_matrix_UB_23      0.0048428000
_diffrn_orient_matrix_UB_31      -0.0199864000
_diffrn_orient_matrix_UB_32      0.0009822000
_diffrn_orient_matrix_UB_33      -0.0502384000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1918
_diffrn_reflns_av_unetI/netI     0.1449
_diffrn_reflns_Laue_measured_fraction_full 0.947
_diffrn_reflns_Laue_measured_fraction_max 0.947
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            17899
_diffrn_reflns_point_group_measured_fraction_full 0.854
_diffrn_reflns_point_group_measured_fraction_max 0.854
_diffrn_reflns_theta_full        52.660
_diffrn_reflns_theta_max         52.660
_diffrn_reflns_theta_min         3.448
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.217
_exptl_absorpt_correction_T_max  0.895
_exptl_absorpt_correction_T_min  0.674
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.27b (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.268
_exptl_crystal_description       plate
_exptl_crystal_F_000             4768
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.071
_exptl_crystal_size_min          0.067
_refine_diff_density_max         0.976
_refine_diff_density_min         -0.535
_refine_diff_density_rms         0.114
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.056(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1167
_refine_ls_number_reflns         11917
_refine_ls_number_restraints     324
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.1235
_refine_ls_R_factor_gt           0.0866
_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^)+(0.1536P)^2^+35.4792P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2179
_refine_ls_wR_factor_ref         0.2464
_reflns_Friedel_coverage         0.650
_reflns_Friedel_fraction_full    0.743
_reflns_Friedel_fraction_max     0.743
_reflns_number_gt                8807
_reflns_number_total             11917
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc09537f2.cif
_cod_data_source_block           zk-m075b_twin1_hklf4
_cod_depositor_comments          'Adding full bibliography for 7121056.cif.'
_cod_original_cell_volume        12133.6(12)
_cod_database_code               7121056
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C52 H52 Cl2 N8 O11 P2 Pd'
_chemical_oxdiff_usercomment     'Sacha's crystal'
_diffrn_oxdiff_ac3_digest_frames
;
017c3f63cb53c1bf843ad14a41c1fcafa300464892d
;
_diffrn_oxdiff_ac3_digest_hkl
;
01e1f0d39837fb4db0299aa36ec68dc0a0ce18
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C028 \\sim C02D \\sim C02F \\sim C023 \\sim C019 \\sim C01T: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C01Y \\sim C02E \\sim C03I \\sim C018 \\sim C014 \\sim C02Y: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C01S \\sim C01J \\sim C03A \\sim C03X \\sim C03H \\sim C03N: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C02F \\sim C02D \\sim C028 \\sim C01T \\sim C019 \\sim C023: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C020 \\sim C03E \\sim C02A \\sim C02U \\sim C01V \\sim C02S: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C03H \\sim C03N \\sim C01S \\sim C01J \\sim C03A \\sim C03X: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C023 \\sim C019 \\sim C01T \\sim C028 \\sim C02D \\sim C02F: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C01V \\sim C02U \\sim C02A \\sim C03E \\sim C020 \\sim C02S: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C039 \\sim C01C \\sim C03R \\sim C02O \\sim C02W \\sim C031: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C03O \\sim C034 \\sim C02N \\sim C022 \\sim C03G \\sim C01A: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C019 \\sim C01T \\sim C028 \\sim C02D \\sim C02F \\sim C023: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C00U \\sim C02Q \\sim C00V \\sim C01G \\sim C02X \\sim C01N: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C03H) = Uanis(C03X) = Uanis(C03A) = Uanis(C01J) = Uanis(C01S) =
Uanis(C03N)
Uanis(C020) = Uanis(C03E) = Uanis(C02A) = Uanis(C02U) = Uanis(C01V) =
Uanis(C02S)
3. Rigid body (RIGU) restrains
 C03V, C03T, C046, C048, C03S, C03M
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C03C, C03D, C03B, C03W, C047, C03P
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Ternary CH refined with riding coordinates:
 C01O(H01O), C024(H024), C025(H025), C02C(H02C), C02T(H02T), C02V(H02V),
 C032(H032), C035(H035)
4.b Aromatic/amide H refined with riding coordinates:
 N00F(H00F), N00G(H00G), N00J(H00J), N00L(H00L), N00M(H00M), N00O(H00O),
 C00U(H00U), C00V(H00V), N00W(H00W), N015(H015), C018(H018), C03I(H03I),
 C02E(H02E), C01Y(H01Y), C02Y(H02Y), C01F(H01F), C01L(H01L), C01M(H01M),
 C01Q(H01Q), C01U(H01U), C03E(H03Q), C02A(H02F), C02U(H02U), C01V(H01V),
 C02S(H02S), C021(H021), C028(H028), C019(H019), C023(H023), C02F(H02G),
 C02D(H02H), C02B(H02I), C02N(H02N), C022(H022), C03G(H03G), C03O(H03O),
 C034(H034), C02P(H02P), C02X(H02X), C02Z(H02Z), C01C(H01C), C03R(H03R),
 C02O(H02O), C02W(H02W), C031(H031), C03D(H03S), C03B(H03T), C03W(H03W),
 C047(H047), C03P(H03U), C03M(H03Z), C03T(H03), C046(H046), C048(H048),
 C03S(H0AA), C03H(H03N), C03X(H03X), C03A(H03P), C01J(H01J), C01S(H01S)
4.c Fitted hexagon refined as free rotating group:
 C018(C03I,C02E,C01Y,C02Y,C014), C020(C03E,C02A,C02U,C01V,C02S), C028(C01T,
 C019,C023,C02F,C02D), C02N(C022,C03G,C01A,C03O,C034), C039(C01C,C03R,C02O,C02W,
 C031), C03C(C03D,C03B,C03W,C047,C03P), C03M(C03V,C03T,C046,C048,C03S),
 C03N(C03H,C03X,C03A,C01J,C01S)
4.d X=CH2 refined with riding coordinates:
 N00S(H00A,H00B), N00X(H00C,H00D), N01D(H01D,H01E), N01P(H01G,H01H), N01W(H01I,
 H01K), N01X(H01A,H01B), N030(H03A,H03B), N03Q(H1AA,HA)
4.e Idealised Me refined as rotating group:
 C02G(H02A,H02B,H02D), C02J(H02J,H02K,H02L), C033(H03C,H03D,H03E), C03F(H03F,
 H03H,H03J), C03J(H03V,H03Y,H), C03K(H03K,H03L,H03M), C03Y(H2AA,HB,HC),
 C042(H04A,H04B,H04C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.578
_oxdiff_exptl_absorpt_empirical_full_min 0.600
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2
_twin_special_details
;
Component 2 rotated by -178.8273\% 
 around [1.00 0.09 0.03] (reciprocal) or [1.00 0.07 0.01] (direct)
;