Crystal structure of (diaqua-bis(phenanthroline-K 2 N,N′)-tetrakis(m 2-3,4,5,6-tetrafluorophthalato-K 4 O,O:O′:O″;K 2 O:O′)dierbium (III) phenanthroline (1/2), C80H38Er2F16N8O18
Song, Jun-Ya; Zhang, Xiao-Yu; Zhang, Chun-Li; Zhao, Bei-Bei; Huang, Shi-Jie; Liu, Xinfang; Zeitschrift für Kristallographie - New Crystal Structures 238 (2023) 441–443; doi:10.1515/ncrs-2023-0023

data_8107463
_publ_section_title
;
 Crystal structure of (diaqua-bis(phenanthroline-K 2
 N,N&#x2032;)-tetrakis(m 2-3,4,5,6-tetrafluorophthalato-K 4
 O,O:O&#x2032;:O&#x2033;;K 2 O:O&#x2032;)dierbium (III) phenanthroline
 (1/2), C80H38Er2F16N8O18
;
_journal_issue                   3
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              441
_journal_page_last               443
_journal_paper_doi               10.1515/ncrs-2023-0023
_journal_volume                  238
_journal_year                    2023
_chemical_formula_moiety         'C56 H22 Er2 F16 N4 O18, 2(C12 H8 N2)'
_chemical_formula_sum            'C80 H38 Er2 F16 N8 O18'
_chemical_formula_weight         2037.70
_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                102.660(2)
_cell_angle_beta                 98.047(3)
_cell_angle_gamma                105.509(3)
_cell_formula_units_Z            1
_cell_length_a                   11.4228(4)
_cell_length_b                   12.6712(3)
_cell_length_c                   13.2663(4)
_cell_measurement_reflns_used    9648
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.9010
_cell_measurement_theta_min      3.9040
_cell_volume                     1764.54(10)
_computing_cell_refinement       'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_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_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0584
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.854
_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    -42.00   0.00   1.00    2.15    --  -15.84 -77.00  30.00   42
  2  \w    -21.00  10.00   1.00    2.15    --  -15.84 -77.00  90.00   31
  3  \w    -43.00 -13.00   1.00    2.15    --  -15.84  77.00-180.00   30
  4  \w     51.00  77.00   1.00    2.15    --   17.09 178.00  60.00   26
  5  \w    -46.00  19.00   1.00    2.15    --   17.09 -57.00-150.00   65
  6  \w    -48.00  24.00   1.00    2.15    --   17.09 -57.00  90.00   72
  7  \w     -8.00  39.00   1.00    2.15    --   17.09  77.00 -60.00   47
  8  \w     -1.00  83.00   1.00    2.15    --   17.09  38.00  30.00   84
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0617830000
_diffrn_orient_matrix_UB_12      0.0022805000
_diffrn_orient_matrix_UB_13      0.0201160000
_diffrn_orient_matrix_UB_21      -0.0188134000
_diffrn_orient_matrix_UB_22      -0.0170064000
_diffrn_orient_matrix_UB_23      0.0442431000
_diffrn_orient_matrix_UB_31      -0.0132478000
_diffrn_orient_matrix_UB_32      -0.0578225000
_diffrn_orient_matrix_UB_33      -0.0279467000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0337
_diffrn_reflns_av_unetI/netI     0.0530
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.854
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15821
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.854
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.143
_diffrn_reflns_theta_min         3.374
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.488
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92930
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.121a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.918
_exptl_crystal_description       block
_exptl_crystal_F_000             998
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.850
_refine_diff_density_min         -0.911
_refine_diff_density_rms         0.105
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     561
_refine_ls_number_reflns         8127
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0348
_refine_ls_R_factor_gt           0.0311
_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^)+(0.0268P)^2^+0.0368P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0644
_refine_ls_wR_factor_ref         0.0668
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7495
_reflns_number_total             8127
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2023-0023_suppl_001.cif
_cod_data_source_block           er-fi_auto
_cod_database_code               8107463
_chemical_oxdiff_formula         'C1 H1 N1 Er1 F1 O1 '
_shelx_estimated_absorpt_t_max   0.663
_shelx_estimated_absorpt_t_min   0.636
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2.a Rotating group:
 O9(H9A,H9B)
2.b Aromatic/amide H refined with riding coordinates:
 C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23),
 C24(H24), C29(H29), C30(H30), C31(H31), C32(H32), C33(H33), C34(H34), C35(H35),
  C36(H36)
2.c Idealised tetrahedral OH refined as rotating group:
 O2(H2)
;
_shelx_res_checksum              83161
_shelx_hkl_checksum              81688
_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 1.149
_oxdiff_exptl_absorpt_empirical_full_min 0.866