The crystal structure of catena-[diaqua-(4-acetylphenoxyacetato-κ 2 O,O)-bis(4-acetylphenoxyacetato-κ 3 O,O:O)-dihydrate-lanthanum(III)]–4,4′-bipyridine (2/1), C35H35NO14La
Ying, Liu; Xi-Hai, Yan; Yuan-Fang, Wang; Xi-Shi, Tai; Zeitschrift für Kristallographie - New Crystal Structures 238 (2023) 1061–1063; doi:10.1515/ncrs-2023-0301

data_8107660
_publ_section_title
;
 The crystal structure of catena-[diaqua-(4-acetylphenoxyacetato-\k 2
 O,O)-bis(4-acetylphenoxyacetato-\k 3
 O,O:O)-dihydrate-lanthanum(III)]--4,4&#x2032;-bipyridine (2/1),
 C35H35NO14La
;
_journal_issue                   6
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              1061
_journal_page_last               1063
_journal_paper_doi               10.1515/ncrs-2023-0301
_journal_volume                  238
_journal_year                    2023
_chemical_formula_moiety         'C30 H31 La O14, C5 H4 N'
_chemical_formula_sum            'C35 H35 La N O14'
_chemical_formula_weight         832.55
_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
_cell_angle_alpha                115.2310(10)
_cell_angle_beta                 97.4010(10)
_cell_angle_gamma                95.4830(10)
_cell_formula_units_Z            2
_cell_length_a                   9.06760(10)
_cell_length_b                   13.6139(2)
_cell_length_c                   15.5964(2)
_cell_measurement_reflns_used    14858
_cell_measurement_temperature    296.13(10)
_cell_measurement_theta_max      76.9300
_cell_measurement_theta_min      3.1820
_cell_volume                     1702.65(4)
_computing_cell_refinement       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      296.13(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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     95.00 139.00   0.50    0.10    --  107.75  57.00-120.00   88
  2  \w    138.00 176.00   0.50    0.10    --  107.75  37.00 -30.00   76
  3  \w     98.00 124.00   0.50    0.10    --  107.75  37.00 -30.00   52
  4  \w    115.00 169.00   0.50    0.10    --  107.75  57.00  90.00  108
  5  \w    -40.00  18.00   0.50    0.05    --  -47.70  37.00 -60.00  116
  6  \w    -27.00  26.00   0.50    0.05    --  -47.70  19.00  90.00  106
  7  \w     -4.00  21.00   0.50    0.05    --  -47.70  19.00-150.00   50
  8  \w     83.00 112.00   0.50    0.10    --  107.75-125.00-120.00   58
  9  \w     70.00 110.00   0.50    0.10    --  107.75-125.00 -60.00   80
 10  \w     36.00  61.00   0.50    0.10    --  107.75-125.00 -60.00   50
 11  \w     79.00 112.00   0.50    0.10    --  107.75-125.00  60.00   66
 12  \w     80.00 112.00   0.50    0.10    --  107.75-125.00  90.00   64
 13  \w     37.00  66.00   0.50    0.10    --  107.75-125.00  90.00   58
 14  \w     35.00  87.00   0.50    0.10    --  107.75 -99.00  30.00  104
 15  \w     60.00 108.00   0.50    0.10    --  107.75-112.00 103.00   96
 16  \w     39.00  78.00   0.50    0.10    --  107.75 -99.00   0.00   78
 17  \w     35.00 106.00   0.50    0.10    --  107.75 -99.00 -60.00  142
 18  \w     38.00  64.00   0.50    0.05    --   47.70-112.00 103.00   52
 19  \w     76.00 101.00   0.50    0.10    --  107.75 -99.00 120.00   50
 20  \w     41.00  72.00   0.50    0.10    --  107.75 -99.00 120.00   62
 21  \w     36.00  67.00   0.50    0.10    --  107.75 -77.00 120.00   62
 22  \w     74.00  99.00   0.50    0.10    --  107.75 -77.00 120.00   50
 23  \w     40.00  65.00   0.50    0.10    --  107.75 -57.00   0.00   50
 24  \w     41.00  71.00   0.50    0.10    --  107.75 -77.00-180.00   60
 25  \w     76.00 101.00   0.50    0.10    --  107.75 -77.00-180.00   50
 26  \w     38.00  66.00   0.50    0.10    --  107.75 -57.00 -60.00   56
 27  \w     -4.00  25.00   0.50    0.05    --   47.70 -19.00  90.00   58
 28  \w     36.00  65.00   0.50    0.10    --  107.75 -57.00 120.00   58
 29  \w     35.00  65.00   0.50    0.10    --  107.75 -57.00 150.00   60
 30  \w    104.00 152.00   0.50    0.10    --  107.75 112.00-163.00   96
 31  \w     98.00 148.00   0.50    0.10    --  107.75 125.00 -30.00  100
 32  \w     95.00 146.00   0.50    0.10    --  107.75 125.00  90.00  102
 33  \w    -65.00 -14.00   0.50    0.10    --  -86.25  57.00  90.00  102
 34  \w    -41.00 -13.00   0.50    0.10    --  -86.25  37.00  60.00   56
 35  \w    -41.00 -16.00   0.50    0.10    --  -86.25  37.00 -30.00   50
 36  \w    -42.00 -15.00   0.50    0.10    --  -86.25  37.00-120.00   54
 37  \w    -82.00 -51.00   0.50    0.05    --  -47.70 112.00-163.00   62
 38  \w    -76.00 -51.00   0.50    0.10    --  -86.25 112.00-163.00   50
 39  \w    -83.00 -20.00   0.50    0.10    --  -86.25 125.00-150.00  126
 40  \w    -42.00  -4.00   0.50    0.05    --  -47.70 112.00-163.00   76
 41  \w   -121.00 -43.00   0.50    0.05    --  -47.70 -19.00 -90.00  156
 42  \w   -160.00-123.00   0.50    0.10    --  -86.25 -19.00 -30.00   74
 43  \w   -117.00 -90.00   0.50    0.10    --  -86.25 -19.00 -30.00   54
 44  \w   -154.00 -72.00   0.50    0.10    --  -86.25 -57.00 120.00  164
 45  \w   -107.00 -76.00   0.50    0.05    --  -47.70-125.00 -90.00   62
 46  \w   -126.00 -97.00   0.50    0.10    --  -86.25 -99.00-150.00   58
 47  \w   -136.00 -88.00   0.50    0.10    --  -86.25-112.00 103.00   96
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0573278000
_diffrn_orient_matrix_UB_12      0.0068035000
_diffrn_orient_matrix_UB_13      -0.0943685000
_diffrn_orient_matrix_UB_21      0.0313264000
_diffrn_orient_matrix_UB_22      0.1267091000
_diffrn_orient_matrix_UB_23      0.0546648000
_diffrn_orient_matrix_UB_31      0.1610401000
_diffrn_orient_matrix_UB_32      0.0007435000
_diffrn_orient_matrix_UB_33      -0.0216348000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0857
_diffrn_reflns_av_unetI/netI     0.0712
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            20535
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        66.598
_diffrn_reflns_theta_max         66.598
_diffrn_reflns_theta_min         3.189
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.325
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.20029
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.624
_exptl_crystal_description       block
_exptl_crystal_F_000             842
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.017
_refine_diff_density_min         -1.598
_refine_diff_density_rms         0.136
_refine_ls_extinction_coef       0.0023(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     466
_refine_ls_number_reflns         6027
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0431
_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^)+(0.0644P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1046
_refine_ls_wR_factor_ref         0.1059
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5689
_reflns_number_total             6027
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2023-0301_suppl_001.cif
_cod_data_source_block           5-1
_cod_database_code               8107660
_chemical_oxdiff_formula         'C H N O La'
_shelx_estimated_absorpt_t_max   0.425
_shelx_estimated_absorpt_t_min   0.307
_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.a Rotating group:
 O13(H13A,H13B), O14(H14A,H14B)
2.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C12(H12A,H12B), C22(H22A,H22B)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C6(H6), C14(H14), C15(H15), C17(H17), C18(H18), C24(H24),
 C25(H25), C27(H27), C28(H28), C31(H31), C32(H32), C33(H33), C34(H34), C35(H35)
2.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C19(H19A,H19B,H19C), C30(H30A,H30B,H30C)
;
_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 4.753
_oxdiff_exptl_absorpt_empirical_full_min 0.334