The crystal structure of aqua-bis{2-bromo-6-((2-(2-phenylacetyl)hydrazineylidene)methyl)phenolato-κ3 N,O,O′}-dimethylformamide-κ1 O-erbium(III) chloride – dimethylformamide – water (1/2/1), C39H49N7O9Br2ClEr
Wang, Li-Hua; Tai, Hao-Wen; Song, Gui-Quan; Tai, Xi-Shi; Zeitschrift für Kristallographie - New Crystal Structures 238 (2023) 437–439; doi:10.1515/ncrs-2023-0014

data_8107462
_publ_section_title
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 The crystal structure of
 aqua-bis{2-bromo-6-((2-(2-phenylacetyl)hydrazineylidene)methyl)phenolato-\k3
 N,O,O&#x2032;}-dimethylformamide-\k1 O-erbium(III) chloride --
 dimethylformamide -- water&#x00A0;(1/2/1), C39H49N7O9Br2ClEr
;
_journal_issue                   3
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              437
_journal_page_last               439
_journal_paper_doi               10.1515/ncrs-2023-0014
_journal_volume                  238
_journal_year                    2023
_chemical_formula_moiety         'C84 H70 N4 O24 Yb2, 4(H2 O)'
_chemical_formula_sum            'C84 H78 N4 O28 Yb2'
_chemical_formula_weight         1937.58
_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                70.873(2)
_cell_angle_beta                 80.281(2)
_cell_angle_gamma                65.810(2)
_cell_formula_units_Z            1
_cell_length_a                   12.3164(9)
_cell_length_b                   12.7581(9)
_cell_length_c                   14.5023(11)
_cell_measurement_reflns_used    9859
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      24.67
_cell_measurement_theta_min      2.39
_cell_volume                     1962.4(3)
_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 0.987
_diffrn_measured_fraction_theta_max 0.987
_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  0.0636
_diffrn_reflns_av_unetI/netI     0.0543
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_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            44757
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.081
_diffrn_reflns_theta_max         25.081
_diffrn_reflns_theta_min         2.131
_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    2.456
_exptl_absorpt_correction_T_max  0.802
_exptl_absorpt_correction_T_min  0.731
_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    1.640
_exptl_crystal_density_meas      .
_exptl_crystal_description       block
_exptl_crystal_F_000             974
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.537
_refine_diff_density_min         -0.707
_refine_diff_density_rms         0.116
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     536
_refine_ls_number_reflns         6893
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0519
_refine_ls_R_factor_gt           0.0383
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0219P)^2^+5.1294P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0717
_refine_ls_wR_factor_ref         0.0765
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5870
_reflns_number_total             6893
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2023-0014_suppl.cif
_cod_data_source_block           01
_cod_database_code               8107462
_shelx_estimated_absorpt_t_max   0.809
_shelx_estimated_absorpt_t_min   0.725
_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. Uiso/Uaniso restraints and constraints
Uanis(O14) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3.a Free rotating group:
 O14(H14C,H14D), O13(H13A,H13B)
3.b Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C24(H24A,H24B), C33(H33A,H33B)
3.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C10(H10), C11(H11), C12(H12),
 C16(H16), C17(H17), C19(H19), C20(H20), C26(H26), C27(H27), C29(H29), C30(H30),
  C35(H35), C36(H36), C38(H38), C39(H39)
3.d Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C31(H31A,H31B,H31C), C41(H41A,H41B,H41C)
;
_olex2_submission_special_instructions 'No special instructions were received'