Fluorescence properties of heterotrinuclear Zn(ii)‒M(ii) (M = Ca, Sr and Ba) bis(salamo)-type complexes
Wang, Li; Li, Xiao-Yan; Zhao, Qing; Li, Li-Hong; Dong, Wen-Kui; RSC Adv. 7 (2017) 48730–; doi:10.1039/C7RA08789F

data_7229358
_publ_section_title
;
 Fluorescence properties of heterotrinuclear Zn(ii)--M(ii) (M = Ca, Sr and
 Ba) bis(salamo)-type complexes
;
_journal_issue                   77
_journal_name_full               'RSC Adv.'
_journal_page_first              48730
_journal_paper_doi               10.1039/C7RA08789F
_journal_volume                  7
_journal_year                    2017
_chemical_formula_moiety         'C38 H38 Ca N4 O14 Zn2, C H Cl3'
_chemical_formula_sum            'C39 H39 Ca Cl3 N4 O14 Zn2'
_chemical_formula_weight         1064.91
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-05-05
_audit_creation_method
;
Olex2 1.2
(compiled 2014.11.28 svn.r3106 for OlexSys, GUI svn.r4959)
;
_audit_update_record
;
2017-07-25 deposited with the CCDC.
2017-10-06 downloaded from the CCDC.
;
_cell_angle_alpha                84.531(12)
_cell_angle_beta                 80.178(12)
_cell_angle_gamma                86.928(11)
_cell_formula_units_Z            2
_cell_length_a                   12.4374(17)
_cell_length_b                   12.9596(18)
_cell_length_c                   13.3757(19)
_cell_measurement_reflns_used    2390
_cell_measurement_temperature    295.42(10)
_cell_measurement_theta_max      23.1120
_cell_measurement_theta_min      3.4180
_cell_volume                     2113.1(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      295.42(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0733
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega   -1.00   87.50   1.5000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       20.4291   57.0000  120.0000 59

  2 omega   12.00   42.00   1.5000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       20.4291  -57.0000  120.0000 20

  3 omega   -3.00   37.50   1.5000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       20.4291  -38.0000  -30.0000 27

  4 omega  -20.00   20.50   1.5000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.9916  -99.0000  -90.0000 27

  5 omega   -4.00   86.00   1.5000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       20.4291   38.0000  -90.0000 60

  6 omega  -47.00   50.50   1.5000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       20.4291  -77.0000  -30.0000 65
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0290814000
_diffrn_orient_matrix_UB_12      -0.0310754000
_diffrn_orient_matrix_UB_13      -0.0373050000
_diffrn_orient_matrix_UB_21      0.0059290000
_diffrn_orient_matrix_UB_22      -0.0404863000
_diffrn_orient_matrix_UB_23      0.0384903000
_diffrn_orient_matrix_UB_31      -0.0497378000
_diffrn_orient_matrix_UB_32      -0.0205565000
_diffrn_orient_matrix_UB_33      -0.0067501000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0606
_diffrn_reflns_av_unetI/netI     0.1220
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            14901
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         3.27
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.519
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94128
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.674
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.727
_refine_diff_density_min         -0.534
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     572
_refine_ls_number_reflns         8331
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.1055
_refine_ls_R_factor_gt           0.0584
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0220P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0913
_refine_ls_wR_factor_ref         0.1181
_reflns_number_gt                5285
_reflns_number_total             8331
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7ra08789f2.cif
_cod_data_source_block           d673_2
_cod_database_code               7229358
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.a Ternary CH refined with riding coordinates:
 C39(H39)
2.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C10(H10A,H10B), C11(H11A,H11B), C24(H24A,H24B), C25(H25A,H25B),
 C34(H34A,H34B)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C7(H7), C12(H12), C18(H18), C19(H19), C20(H20),
 C21(H21), C23(H23), C26(H26), C30(H30), C31(H31), C32(H32)
2.d Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C33(H33A,H33B,H33C), C36(H36A,H36B,H36C), C38(H38A,H38B,H38C)
;
_olex2_date_sample_data_collection 2015-04-22
_olex2_submission_special_instructions 'No special instructions were received'