#------------------------------------------------------------------------------
#$Date: 2019-11-17 06:58:33 +0200 (Sun, 17 Nov 2019) $
#$Revision: 228531 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/25/7122554.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7122554
loop_
_publ_author_name
'Lin, Qi'
'Gao, Lei'
'Kauffmann, Brice'
'Zhang, Jiajia'
'Ma, Chunmiao'
'Luo, Dan'
'Gan, Quan'
_publ_section_title
;
 Helicity adaptation within a quadruply stranded helicate by
 encapsulation.
;
_journal_issue                   95
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              13447
_journal_page_last               13450
_journal_paper_doi               10.1039/c8cc07932c
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         'C128 H124 F4 N24 O16 Pd2, B12 F12, 2(B F4)'
_chemical_formula_sum            'C128 H124 B14 F24 N24 O16 Pd2'
_chemical_formula_weight         3074.64
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-09-12
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-09-12 deposited with the CCDC.
2018-11-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.821(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.8811(9)
_cell_length_b                   22.8682(11)
_cell_length_c                   44.582(2)
_cell_measurement_reflns_used    34000
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      67.6080
_cell_measurement_theta_min      2.6500
_cell_volume                     20197.3(16)
_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_temperature      100.15
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'XtaLAB AFC12:kappa single'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0953
_diffrn_reflns_av_unetI/netI     0.0725
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            189676
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        59.275
_diffrn_reflns_theta_max         59.275
_diffrn_reflns_theta_min         1.989
_exptl_absorpt_coefficient_mu    2.051
_exptl_absorpt_correction_T_max  0.9
_exptl_absorpt_correction_T_min  0.6
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.011
_exptl_crystal_description       block
_exptl_crystal_F_000             6264
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.851
_refine_diff_density_min         -0.723
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.147
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1889
_refine_ls_number_reflns         29134
_refine_ls_number_restraints     85
_refine_ls_restrained_S_all      1.156
_refine_ls_R_factor_all          0.1294
_refine_ls_R_factor_gt           0.1030
_refine_ls_shift/su_max          2.859
_refine_ls_shift/su_mean         0.011
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2969
_refine_ls_wR_factor_ref         0.3188
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18956
_reflns_number_total             29134
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8cc07932c2.cif
_cod_data_source_block           xx_a
_cod_depositor_comments
'Adding full bibliography for 7122551--7122554.cif.'
_cod_original_cell_volume        20197.2(17)
_cod_database_code               7122554
_shelx_shelxl_version_number     2017/1
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.821
_shelx_estimated_absorpt_t_min   0.685
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C59-C44
 1.54 with sigma of 0.02
 C13-C59
 1.54 with sigma of 0.02
 C054-C05K
 2.6 with sigma of 0.02
 C22-C50
 1.6 with sigma of 0.02
 C21-C71
 2.4 with sigma of 0.002
 C50-C71
 1.5 with sigma of 0.002
 C50-C21
 1.5 with sigma of 0.002
 C59-C52
 1.5 with sigma of 0.002
3. Rigid bond restraints
 C44, C59
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C50, C71
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C13, C59
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C04J, C6AA
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C21, C50
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C02T, C03C
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C038, C03X
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 F00Y, B05E
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 F01K, B04R
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 B050, B056
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C04F, C04U
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C22, C50
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C03T, C045
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 O1, C058
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 O5, C22
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 O1, C13
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 O5, C7AA
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 O02P, C04C
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C02H, C02R
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C04J, C05V
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C04L, C7AA
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C52, C59
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C04T, C05P
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
4. Uiso/Uaniso restraints and constraints
Uanis(C59) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C13) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C22) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C50) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C52) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C44) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O5) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O02P) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C7AA) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5.a Ternary CH refined with riding coordinates:
 C04J(H04J), C04M(H04M), C04N(H04N), C04T(H04T), C04U(H04U), C05B(H05L),
 C59(H59), C50(H50)
5.b Secondary CH2 refined with riding coordinates:
 C03W(H03B,H03C), C043(H04A,H04B), C04D(H04C,H04D), C04F(H04E,H04F), C04V(H04R,
 H04S), C052(H05A,H05B), C13(H13A,H13B), C22(H22A,H22B)
5.c Aromatic/amide H refined with riding coordinates:
 N00G(H00G), N00J(H00J), N00P(H00P), N00U(H00U), N00X(H00X), C019(H019),
 C01A(H01A), C01F(H01F), N01G(H01G), C01J(H01J), N01M(H01M), C01X(H01X),
 C01Y(H01Y), N022(H022), C025(H025), C029(H029), C02E(H02E), C02F(H02F),
 C02I(H02I), C02Q(H02Q), C02S(H02S), C02T(H02T), C02V(H02V), C02Y(H02Y),
 C02Z(H02Z), C033(H033), C035(H035), C039(H039), C03A(H03A), C03E(H03E),
 C03G(H03G), C03H(H03H), C03I(H03I), C03J(H03J), C03K(H03K), C03M(H03M),
 C03N(H03N), C03P(H03P), C03Q(H03Q), C03S(H03S), C03T(H03T), C03U(H03U),
 C03X(H03X), C03Z(H03Z), C040(H040), C045(H045), C046(H046), C048(H048),
 C04K(H04K), C04L(H04L), C053(H053), C05M(H05S)
5.d Idealised Me refined as rotating group:
 C04O(H04G,H04H,H04I), C04S(H04O,H04P,H04Q), C054(H05C,H05D,H05E), C055(H05F,
 H05G,H05H), C05A(H05I,H05J,H05K), C05C(H05M,H05N,H05O), C05K(H05P,H05Q,H05R),
 C05N(H05T,H05U,H05V), C05P(H05W,H05X,H05Y), C05Q(H05Z,H,HA), C05V(H05,HB,HC),
 C6AA(H6AA,H6AB,H6AC), C44(H44A,H44B,H44C), C52(H52A,H52B,H52C), C21(H21A,H21B,
 H21C), C71(H71A,H71B,H71C)
;
