Crystal structure of bis(2,2′-bipyridine-κ2N,N′)-tetrakis(μ2-3-(phenylsulfonamido)propanoato-κ2O:O′)-bis(3-(phenylsulfonamido)propanoato-κ2O,O′)digadolinium(III) – 2,2′-bipyridine (1/1), C84H84Gd2N12O24S6
Deng, Tao-Li; Liu, Zheng-Jun; Chen, Xiao-Miao; Liu, Xue-Mei; Zeitschrift für Kristallographie - New Crystal Structures 234 (2019) 1189–1191; doi:10.1515/ncrs-2019-0318

data_8105974
_publ_section_title
;
 Crystal structure of
 bis(2,2&#x2032;-bipyridine-\k2N,N&#x2032;)-tetrakis(\m2-3-(phenylsulfonamido)propanoato-\k2O:O&#x2032;)-bis(3-(phenylsulfonamido)propanoato-\k2O,O&#x2032;)digadolinium(III)
 -- 2,2&#x2032;-bipyridine (1/1), C84H84Gd2N12O24S6
;
_journal_issue                   6
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              1189
_journal_page_last               1191
_journal_paper_doi               10.1515/ncrs-2019-0318
_journal_volume                  234
_journal_year                    2019
_chemical_formula_moiety         'C74 H76 Gd2 N10 O24 S6, C10 H8 N2'
_chemical_formula_sum            'C84 H84 Gd2 N12 O24 S6'
_chemical_formula_weight         2152.49
_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     iterative
_cell_angle_alpha                89.635(3)
_cell_angle_beta                 82.334(3)
_cell_angle_gamma                69.794(3)
_cell_formula_units_Z            1
_cell_length_a                   9.733(2)
_cell_length_b                   11.3610(8)
_cell_length_c                   21.4970(3)
_cell_measurement_reflns_used    2939
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20.962
_cell_measurement_theta_min      2.252
_cell_volume                     2208.8(5)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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      293(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0505
_diffrn_reflns_av_unetI/netI     0.0889
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            15497
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.647
_exptl_absorpt_coefficient_mu    1.712
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5566
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
'SADABS-2014/3 (Bruker,2014/3) was used for absorption 
correction. wR2(int) was 0.0848 before and 0.0465 after 
correction. The Ratio of minimum to maximum transmission 
is 0.7465. The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.618
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.919
_refine_diff_density_min         -0.673
_refine_diff_density_rms         0.118
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     577
_refine_ls_number_reflns         7752
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.0706
_refine_ls_R_factor_gt           0.0467
_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^)+(0.0362P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0862
_refine_ls_wR_factor_ref         0.0925
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6039
_reflns_number_total             7752
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2019-0318_suppl.cif
_cod_data_source_block           a
_cod_database_code               8105974
_shelx_estimated_absorpt_t_max   0.674
_shelx_estimated_absorpt_t_min   0.610
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C13(H13A,H13B), C21(H21A,H21B), C22(H22A,H22B), C30(H30A,
 H30B), C31(H31A,H31B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C15(H15),
 C16(H16), C17(H17), C18(H18), C19(H19), C24(H24), C25(H25), C26(H26), C27(H27),
  C28(H28), C33(H33), C34(H34), C35(H35), C36(H36), C38(H38), C39(H39),
 C40(H40), C41(H41), C85(H85), N3(H3A), N4(H4A), N5(H5)
;