Synthesis and crystal structure of bis(μ2-acetato-κ2 O:O′)-bis{μ2-4-chloro-2-(8-(4-(diethylamino)-2-oxidophenyl)-3,6-dioxa-2,7-diazaocta-1,7-dien-1-yl)phenolato-κ6 O:O,N,N′,O′:O′}trizinc(II), C44H49Cl2N6O12Zn3
Li, Li; Hao, Jing; Lan, Peng-Fei; Dong, Wen-Kui; Zeitschrift für Kristallographie - New Crystal Structures 232 (2017) 877–879; doi:10.1515/ncrs-2017-0037

data_8106707
_publ_section_title
;
 Synthesis and crystal structure of bis(\m2-acetato-\k2
 O:O&#x2032;)-bis{\m2-4-chloro-2-(8-(4-(diethylamino)-2-oxidophenyl)-3,6-dioxa-2,7-diazaocta-1,7-dien-1-yl)phenolato-\k6
 O:O,N,N&#x2032;,O&#x2032;:O&#x2032;}trizinc(II), C44H49Cl2N6O12Zn3
;
_journal_issue                   6
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              877
_journal_page_last               879
_journal_paper_doi               10.1515/ncrs-2017-0037
_journal_volume                  232
_journal_year                    2017
_chemical_formula_moiety         'C44 H50 Cl2 N6 O12 Zn3'
_chemical_formula_sum            'C44 H50 Cl2 N6 O12 Zn3'
_chemical_formula_weight         1121.91
_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
_cell_angle_alpha                72.539(8)
_cell_angle_beta                 82.872(7)
_cell_angle_gamma                72.157(8)
_cell_formula_units_Z            2
_cell_length_a                   9.7387(8)
_cell_length_b                   13.7034(12)
_cell_length_c                   20.2498(16)
_cell_measurement_reflns_used    2114
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.9890
_cell_measurement_theta_min      3.6810
_cell_volume                     2452.3(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.0733
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_details
;
  1 omega  -10.00   24.80   1.2000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.3571  -99.0000 -180.0000 29

  2 omega  -49.00   39.80   1.2000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       19.6383  -57.0000 -120.0000 74

  3 omega   37.00   61.00   1.2000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       19.6383  -99.0000   30.0000 20

  4 omega    0.00   92.40   1.2000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       19.6383   38.0000   30.0000 77

  5 omega   -5.00   31.00   1.2000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       19.6383   38.0000  120.0000 30

  6 omega   35.00   71.00   1.2000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       19.6383   38.0000  120.0000 30

  7 omega   -2.00   88.00   1.2000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       19.6383   57.0000 -180.0000 75
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0293874000
_diffrn_orient_matrix_UB_12      -0.0385815000
_diffrn_orient_matrix_UB_13      0.0241241000
_diffrn_orient_matrix_UB_21      0.0702137000
_diffrn_orient_matrix_UB_22      -0.0303936000
_diffrn_orient_matrix_UB_23      0.0116350000
_diffrn_orient_matrix_UB_31      -0.0082516000
_diffrn_orient_matrix_UB_32      0.0281260000
_diffrn_orient_matrix_UB_33      0.0251528000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1192
_diffrn_reflns_av_unetI/netI     0.2465
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            16652
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.022
_diffrn_reflns_theta_min         3.378
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.630
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86010
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.519
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.571
_refine_diff_density_min         -1.169
_refine_diff_density_rms         0.133
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.820
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     629
_refine_ls_number_reflns         9456
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      0.820
_refine_ls_R_factor_all          0.1894
_refine_ls_R_factor_gt           0.0600
_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^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0798
_refine_ls_wR_factor_ref         0.1392
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4735
_reflns_number_total             9456
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2017-0037_suppl.cif
_cod_data_source_block           d533
_cod_database_code               8106707
_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
2. Restrained distances
 C40-C39
 1.45 with sigma of 0.02
 N6-C39
 1.45 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C40) \\sim Ueq, Uanis(C39) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C39) \\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C40') \\sim Ueq, Uanis(C39')
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: C39(0.5) H39A(0.5) H39B(0.5) C40(0.5) H40A(0.5) H40B(0.5)
 H40C(0.5) C39'(0.5) H39C(0.5) H39D(0.5) C40'(0.5) H40D(0.5) H40E(0.5) H40F(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C17(H17A,H17B), C19(H19A,H19B), C28(H28A,H28B),
 C29(H29A,H29B), C37(H37A,H37B), C39(H39A,H39B), C39'(H39C,H39D)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C7(H7), C10(H10), C13(H13), C15(H15), C16(H16),
 C22(H22), C23(H23), C25(H25), C27(H27), C30(H30), C33(H33), C35(H35), C36(H36)
5.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C38(H38A,H38B,H38C), C42(H42A,H42B,
 H42C), C44(H44A,H44B,H44C), C40(H40A,H40B,H40C), C40'(H40D,H40E,H40F)
;
_shelx_res_checksum              76850
_shelx_hkl_checksum              90436
_olex2_date_sample_data_collection 1416801822.64
_olex2_submission_special_instructions 'No special instructions were received'