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_7229342
_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 H42 N4 Ni2 O16 Sr, 2(C H2 Cl2), 2(C H4 O)'
_chemical_formula_sum            'C42 H54 Cl4 N4 Ni2 O18 Sr'
_chemical_formula_weight         1249.73
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2016-05-28
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2017-07-15 deposited with the CCDC.
2017-10-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.6620(5)
_cell_length_b                   17.8187(5)
_cell_length_c                   12.4666(3)
_cell_measurement_reflns_used    3354
_cell_measurement_temperature    154.89(10)
_cell_measurement_theta_max      24.1120
_cell_measurement_theta_min      3.8620
_cell_volume                     5256.2(2)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      154.89(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0733
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega   37.00   91.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5854  178.0000   30.0000 54

  2 omega   33.00   66.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5854   57.0000    0.0000 33

  3 omega  -45.00   46.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5854  -38.0000   60.0000 91
;
_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      0.0028601000
_diffrn_orient_matrix_UB_12      -0.0133971000
_diffrn_orient_matrix_UB_13      0.0532983000
_diffrn_orient_matrix_UB_21      0.0190681000
_diffrn_orient_matrix_UB_22      -0.0280003000
_diffrn_orient_matrix_UB_23      -0.0180613000
_diffrn_orient_matrix_UB_31      0.0229535000
_diffrn_orient_matrix_UB_32      0.0249215000
_diffrn_orient_matrix_UB_33      0.0083683000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0500
_diffrn_reflns_av_unetI/netI     0.0613
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            16016
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.019
_diffrn_reflns_theta_min         3.296
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.996
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91236
_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    1.579
_exptl_crystal_description       block
_exptl_crystal_F_000             2560
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.510
_refine_diff_density_min         -0.495
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     329
_refine_ls_number_reflns         5173
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0820
_refine_ls_R_factor_gt           0.0479
_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^)+(0.0308P)^2^+5.6412P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0888
_refine_ls_wR_factor_ref         0.1022
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3648
_reflns_number_total             5173
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ra07826a2.cif
_cod_data_source_block           d846
_cod_database_code               7229342
_chemical_oxdiff_formula         'C27 H15 O6 Cu'
_reflns_odcompleteness_completeness 99.63
_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
2. Restrained distances
 O8-H8
 0.85 with sigma of 0.01
 C19-H8
 1.868573 with sigma of 0.02
 Ni1-H8
 2.685949 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C10(H10A,H10B), C21(H21A,H21B)
3.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C5(H5), C4(H4), C8(H8A), C11(H11), C14(H14), C15(H15)
3.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C)
3.d Idealised tetrahedral OH refined as rotating group:
 O9(H9)
;
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2015-11-23
_olex2_submission_special_instructions 'No special instructions were received'