Crystal structure of bis{μ2-(4-acetyl-phenoxy)acetato-κ2 O:O′}-bis{μ2-(4-acetyl-phenoxy)acetato-κ3 O,O′:O)- bis{(4-acetyl-phenoxy)acetato-κ2 O,O′}-bis(phenanthrolin-κ2 N,N′)didysprosium(III) tetrahydrate, C84H78N4O28Dy2
Wang, Li-Hua; Tai, Hao-Wen; Zhao, Mei-Li; Tai, Xi-Shi; Zeitschrift für Kristallographie - New Crystal Structures 238 (2023) 563–565; doi:10.1515/ncrs-2023-0086

data_8107495
_publ_section_title
;
 Crystal structure of bis{\m2-(4-acetyl-phenoxy)acetato-\k2
 O:O&#x2032;}-bis{\m2-(4-acetyl-phenoxy)acetato-\k3 O,O&#x2032;:O)-
 bis{(4-acetyl-phenoxy)acetato-\k2 O,O&#x2032;}-bis(phenanthrolin-\k2
 N,N&#x2032;)didysprosium(III) tetrahydrate, C84H78N4O28Dy2
;
_journal_issue                   3
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              563
_journal_page_last               565
_journal_paper_doi               10.1515/ncrs-2023-0086
_journal_volume                  238
_journal_year                    2023
_chemical_formula_moiety         'C84 H70 Dy2 N4 O24, 4(H2 O)'
_chemical_formula_sum            'C84 H78 Dy2 N4 O28'
_chemical_formula_weight         1916.50
_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   mixed
_atom_sites_solution_primary     dual
_cell_angle_alpha                70.8520(10)
_cell_angle_beta                 80.2980(10)
_cell_angle_gamma                65.7260(10)
_cell_formula_units_Z            1
_cell_length_a                   12.3134(5)
_cell_length_b                   12.7705(5)
_cell_length_c                   14.5150(6)
_cell_measurement_reflns_used    9932
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      24.99
_cell_measurement_theta_min      2.30
_cell_volume                     1964.05(14)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296.15
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 5.6
_diffrn_detector_type            'Bruker SMART CCD 6000 area detector'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART CCD 6000 area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0757
_diffrn_reflns_av_unetI/netI     0.0573
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            54137
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.119
_diffrn_reflns_theta_max         25.119
_diffrn_reflns_theta_min         2.129
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_target            Mo
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.976
_exptl_absorpt_correction_T_max  0.805
_exptl_absorpt_correction_T_min  0.752
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_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    1.620
_exptl_crystal_density_meas      .
_exptl_crystal_description       block
_exptl_crystal_F_000             966
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.764
_refine_diff_density_min         -0.586
_refine_diff_density_rms         0.115
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     541
_refine_ls_number_reflns         6967
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0545
_refine_ls_R_factor_gt           0.0381
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0127P)^2^+3.8343P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0621
_refine_ls_wR_factor_ref         0.0682
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5875
_reflns_number_total             6967
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2023-0086_suppl_001.cif
_cod_data_source_block           4
_cod_database_code               8107495
_shelx_estimated_absorpt_t_max   0.812
_shelx_estimated_absorpt_t_min   0.756
_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, All O(H,H) groups
2. Restrained distances
 H14C-O14 = O14-H14D
 0.85 with sigma of 0.02
 H14C-H14D
 1.472 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(O13) \\sim Ueq, Uanis(O14) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
4.a Free rotating group:
 O13(H13A,H13B), O14(H14C,H14D)
4.b Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C24(H24A,H24B), C34(H34A,H34B)
4.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C15(H15),
 C16(H16), C18(H18), C19(H19), C26(H26), C27(H27), C29(H29), C30(H30), C36(H36),
  C37(H37), C39(H39), C40(H40)
4.d Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C32(H32A,H32B,H32C), C42(H42A,H42B,H42C)
;
_olex2_submission_special_instructions 'No special instructions were received'