Tri- and hexanuclear heterometallic Ni(ii)‒M(ii) (M = Ca, Sr and Ba) bis(salamo)-type complexes: synthesis, structure and fluorescence properties
Dong, Xiu-Yan; Li, Xiao-Yan; Liu, Ling-Zhi; Zhang, Han; Ding, Yu-Jie; Dong, Wen-Kui; RSC Adv. 7 (2017) 48394–; doi:10.1039/C7RA07826A

data_7229343
_publ_section_title
;
 Tri- and hexanuclear heterometallic Ni(ii)--M(ii) (M = Ca, Sr and Ba)
 bis(salamo)-type complexes: synthesis, structure and fluorescence
 properties
;
_journal_issue                   76
_journal_name_full               'RSC Adv.'
_journal_page_first              48394
_journal_paper_doi               10.1039/C7RA07826A
_journal_volume                  7
_journal_year                    2017
_chemical_formula_moiety         'C38 H44 Ba N4 Ni2 O17, C H4 O'
_chemical_formula_sum            'C39 H48 Ba N4 Ni2 O18'
_chemical_formula_weight         1115.57
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-06-26
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2017-07-15 deposited with the CCDC.
2017-10-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.551(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.8005(3)
_cell_length_b                   15.7041(3)
_cell_length_c                   18.2762(4)
_cell_measurement_reflns_used    6818
_cell_measurement_temperature    294.06(10)
_cell_measurement_theta_max      27.2180
_cell_measurement_theta_min      3.5100
_cell_volume                     4520.62(16)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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_environment      air
_diffrn_ambient_temperature      294.06(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0733
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
  1 omega  -47.00   92.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5854    0.0000   30.0000 139

  2 omega  -18.00   12.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.1479  -99.0000  120.0000 30

  3 omega   57.00   97.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5854  178.0000   90.0000 40

  4 omega   62.00   91.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5854  178.0000 -180.0000 29
;
_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      -0.0411214000
_diffrn_orient_matrix_UB_12      0.0080326000
_diffrn_orient_matrix_UB_13      0.0115312000
_diffrn_orient_matrix_UB_21      0.0016539000
_diffrn_orient_matrix_UB_22      0.0421816000
_diffrn_orient_matrix_UB_23      -0.0135633000
_diffrn_orient_matrix_UB_31      -0.0183354000
_diffrn_orient_matrix_UB_32      -0.0139347000
_diffrn_orient_matrix_UB_33      -0.0346236000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0300
_diffrn_reflns_av_unetI/netI     0.0477
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            17095
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         3.425
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.764
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93646
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.639
_exptl_crystal_description       block
_exptl_crystal_F_000             2264
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.229
_refine_diff_density_min         -0.419
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     600
_refine_ls_number_reflns         7925
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0546
_refine_ls_R_factor_gt           0.0365
_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^)+(0.0287P)^2^+3.8410P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0760
_refine_ls_wR_factor_ref         0.0874
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6205
_reflns_number_total             7925
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ra07826a2.cif
_cod_data_source_block           d848
_cod_database_code               7229343
_shelx_shelxl_version_number     2014/7
_reflns_odcompleteness_completeness 99.72
_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, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O12-H12
 0.87 with sigma of 0.01
 O0AA-H0AD
 0.87 with sigma of 0.01
 C59-H12
 1.884291 with sigma of 0.02
 Ni3-H12
 2.727723 with sigma of 0.02
 C64-H0AD
 1.905039 with sigma of 0.02
 Ni2-H0AD
 2.653174 with sigma of 0.02
 C64-O22 \\sim O22-C0AA
 with sigma of 0.001
3. Rigid bond restraints
 O22, C64, C0AA, O0AA
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
O22 \\sim C64 \\sim C0AA \\sim O0AA: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C0AA) = Uanis(C64)
Uanis(O22) = Uanis(O0AA)
5. Others
 Sof(O22)=Sof(H22)=Sof(C0AA)=Sof(H0AA)=Sof(H0AB)=Sof(H0AC)=1-FVAR(1)
 Sof(C64)=Sof(H64A)=Sof(H64B)=Sof(H64C)=Sof(O0AA)=Sof(H0AD)=FVAR(1)
6.a Rotating group:
 O5(H5A,H5B)
6.b Secondary CH2 refined with riding coordinates:
 C43(H43A,H43B), C50(H50A,H50B), C52(H52A,H52B), C57(H57A,H57B)
6.c Aromatic/amide H refined with riding coordinates:
 C26(H26), C27(H27), C31(H31), C32(H32), C41(H41), C44(H44), C47(H47),
 C49(H49), C51(H51), C54(H54), C55(H55), C56(H56), C61(H61), C63(H63)
6.d Tetrahedral OH refined with riding coordinates:
 O22(H22)
6.e Idealised Me refined as rotating group:
 C42(H42A,H42B,H42C), C46(H46A,H46B,H46C), C48(H48A,H48B,H48C), C58(H58A,H58B,
 H58C), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C), C64(H64A,H64B,H64C),
 C0AA(H0AA,H0AB,H0AC)
6.f Idealised tetrahedral OH refined as rotating group:
 O30(H30)
;
_shelx_res_checksum              69450
_shelx_fab_checksum              35774
_olex2_date_sample_data_collection 2015-11-27
_olex2_submission_special_instructions 'No special instructions were received'