Stereoisomers of metal-organic dimers induced by the steric constraint of dissymmetric terpyridine ligands.
Ma, Jianjun; Yu, Hao; Zhang, Ning; Shi, Junjuan; Li, Jiaqi; Li, Kehuan; Han, Ningxu; Zhang, Houyu; Chang, Junmin; Wang, Ming; Dalton transactions (Cambridge, England : 2003) 54 (2025) 11632–11637; doi:10.1039/d5dt00948k

data_7718989
_publ_section_title
;
 Stereoisomers of metal-organic dimers induced by the steric constraint of
 dissymmetric terpyridine ligands.
;
_journal_issue                   30
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11632
_journal_page_last               11637
_journal_paper_doi               10.1039/d5dt00948k
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C86 H60 N12 O2 Zn2, 4(F6 P), 6(C2 H3 N)'
_chemical_formula_sum            'C98 H78 F24 N18 O2 P4 Zn2'
_chemical_formula_weight         2250.40
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-12-05
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.18 svn.r3501 for OlexSys, GUI svn.r5488)
;
_audit_update_record
;
2022-10-01 deposited with the CCDC.	2025-06-24 downloaded from the CCDC.
;
_cell_angle_alpha                73.950(3)
_cell_angle_beta                 80.852(3)
_cell_angle_gamma                76.310(3)
_cell_formula_units_Z            2
_cell_length_a                   15.4205(10)
_cell_length_b                   15.9087(10)
_cell_length_c                   21.4828(14)
_cell_measurement_reflns_used    9792
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.732
_cell_measurement_theta_min      2.670
_cell_volume                     4896.1(6)
_computing_cell_refinement       'SAINT V8.40A (?, 2016)'
_computing_data_reduction        'SAINT V8.40A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0866
_diffrn_reflns_av_unetI/netI     0.0497
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            188987
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.833
_diffrn_reflns_theta_min         2.518
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.661
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.526
_exptl_crystal_description       block
_exptl_crystal_F_000             2288
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.433
_refine_diff_density_min         -1.304
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1330
_refine_ls_number_reflns         20743
_refine_ls_number_restraints     495
_refine_ls_restrained_S_all      2.109
_refine_ls_R_factor_all          0.1153
_refine_ls_R_factor_gt           0.0698
_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^)+(0.0434P)^2^+21.4341P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1486
_refine_ls_wR_factor_ref         0.1782
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14353
_reflns_number_total             20743
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00948k2.cif
_cod_data_source_block           1_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7718986--7718989.cif.'
_cod_database_code               7718989
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.931
_shelx_estimated_absorpt_t_min   0.919
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H1A,H1B,H1C} of C1
 At 1.5 times of:
  {H04G,H04H,H04I} of C040, {H04D,H04E,H04F} of C042, {H04A,H04B,H04C} of
  C043, {H03C,H03E,H03I} of C03I, {H03L,H03M,H03N} of C03M, {H03P,H03Q,H03R} of
  C03U, {H03S,H03T,H03U} of C03C
2. Shared sites
{P1, P1A}
3. Uiso/Uaniso restraints and constraints
Uanis(F1) = Uanis(F2) = Uanis(F3) = Uanis(F4) = Uanis(F5) = Uanis(F6) =
Uanis(F1A) = Uanis(F2A) = Uanis(F3A) = Uanis(F4A) = Uanis(F5A) = Uanis(F6A)
Uanis(P1) = Uanis(P1A)
4. Same fragment restrains
{P1, F1, F2, F3, F4, F5, F6} sigma for 1-2: 0.02, 1-3: 0.04
{P1A, F1A, F2A, F3A, F4A, F5A, F6A} sigma for 1-2: 0.02, 1-3: 0.04
{P2, F8, F9, F10, F11, F12, F7} sigma for 1-2: 0.02, 1-3: 0.04
as
{P2, F7, F8, F9, F10, F11, F12}
5. Others
 Sof(P1A)=Sof(F1A)=Sof(F2A)=Sof(F3A)=Sof(F4A)=Sof(F5A)=Sof(F6A)=1-FVAR(1)
 Sof(P1)=Sof(F1)=Sof(F2)=Sof(F3)=Sof(F4)=Sof(F5)=Sof(F6)=FVAR(1)
6.a Aromatic/amide H refined with riding coordinates:
 C01B(H01B), C01E(H01E), C01M(H01M), C01O(H01O), C01R(H01R), C01S(H01S),
 C01U(H01U), C01X(H01X), C01Y(H01Y), C01Z(H01Z), C02C(H02C), C02D(H02D),
 C02E(H02E), C02F(H02F), C02G(H02G), C02H(H02H), C02I(H02I), C02J(H02J),
 C02L(H02L), C02O(H02O), C02P(H02P), C02Q(H02Q), C02R(H02R), C02S(H02S),
 C02T(H02T), C02W(H02W), C02X(H02X), C02Y(H02Y), C02Z(H02Z), C03A(H03A),
 C03B(H03B), C03D(H03D), C03F(H03F), C03G(H03G), C03H(H03H), C03J(H03J),
 C03K(H03K), C03N(H03O), C014(H014), C015(H015), C021(H021), C022(H022),
 C023(H023), C024(H024), C026(H026), C027(H027), C030(H030), C031(H031),
 C032(H032), C033(H033), C035(H035), C037(H037), C038(H038), C039(H039)
6.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C03C(H03S,H03T,H03U), C03I(H03C,H03E,H03I), C03M(H03L,H03M,
 H03N), C03U(H03P,H03Q,H03R), C040(H04G,H04H,H04I), C042(H04D,H04E,H04F),
 C043(H04A,H04B,H04C)
;
_shelx_res_checksum              60298
_shelx_hkl_checksum              64593
_olex2_submission_special_instructions 'No special instructions were received'