Alkaline-earth metallacyclic complexes bearing a diborane-bridged tetraamide ligand: synthesis, structure and fluorescence property.
Li, Nan; Zhao, Zifeng; Yu, Chao; Wu, Botao; Bian, Zuqiang; Zhang, Wen-Xiong; Xi, Zhenfeng; Dalton transactions (Cambridge, England : 2003) 48 (2019) 9067–9071; doi:10.1039/c9dt02118c

data_1551211
_publ_section_title
;
 Alkaline-earth metallacyclic complexes bearing a diborane-bridged
 tetraamide ligand: synthesis, structure and fluorescence property.
;
_journal_issue                   25
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9067
_journal_page_last               9071
_journal_paper_doi               10.1039/c9dt02118c
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C44 H86 B2 N16 O4 P4 Sr, C4 H8 O'
_chemical_formula_sum            'C48 H94 B2 N16 O5 P4 Sr'
_chemical_formula_weight         1208.51
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-04-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-04-28 deposited with the CCDC.    2019-06-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.718(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.0218(5)
_cell_length_b                   17.4203(6)
_cell_length_c                   21.4191(7)
_cell_measurement_reflns_used    10780
_cell_measurement_temperature    180.00(10)
_cell_measurement_theta_max      30.7190
_cell_measurement_theta_min      3.7140
_cell_volume                     6240.5(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      180.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -33.00  29.00   0.50   43.00    --   -1.70 -77.00-150.00  124
  2  \w    -32.00   5.00   0.50   43.00    --   -1.70 -82.00  90.00   74
  3  \w      5.00  31.00   0.50   43.00    --   -1.70 -82.00 120.00   52
  4  \w    -87.00 -38.00   0.50   43.00    --    1.90 -37.00-120.00   98
  5  \w     37.00  90.00   0.50   43.00    --    1.90  37.00 -90.00  106
  6  \w    -82.00 -55.00   0.50   43.00    --    1.90 -19.00-180.00   54
  7  \w    -16.00   9.00   0.50   43.00    --    1.90  37.00 -90.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0079457000
_diffrn_orient_matrix_UB_12      -0.0372368000
_diffrn_orient_matrix_UB_13      0.0106873000
_diffrn_orient_matrix_UB_21      0.0168078000
_diffrn_orient_matrix_UB_22      0.0107413000
_diffrn_orient_matrix_UB_23      0.0316306000
_diffrn_orient_matrix_UB_31      -0.0381151000
_diffrn_orient_matrix_UB_32      0.0124986000
_diffrn_orient_matrix_UB_33      0.0047148000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0375
_diffrn_reflns_av_unetI/netI     0.0277
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            31930
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         3.377
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.022
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56368
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.33c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.286
_exptl_crystal_description       block
_exptl_crystal_F_000             2568
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.737
_refine_diff_density_min         -0.396
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     356
_refine_ls_number_reflns         7136
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0363
_refine_ls_R_factor_gt           0.0314
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0513P)^2^+3.9111P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0829
_refine_ls_wR_factor_ref         0.0860
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6436
_reflns_number_total             7136
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02118c2.cif
_cod_data_source_block           4a-THF
_cod_depositor_comments
'Adding full bibliography for 1551209--1551214.cif.'
_cod_database_code               1551211
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C H B O P Sr N'
_shelx_estimated_absorpt_t_max   0.905
_shelx_estimated_absorpt_t_min   0.905
_reflns_odcompleteness_completeness 99.58
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C38(H38a,H38b), C37(H37a,H37b)
2.b Aromatic/amide H refined with riding coordinates:
 N1(H1), C7(H7), C2(H2), C1(H1a), C3(H3), C8(H8), C9(H9)
2.c Idealised Me refined as rotating group:
 C0aa(H0aa,H0ab,H0ac), C13(H13a,H13b,H13c), C23(H23a,H23b,H23c), C4aa(H4aa,
 H4ab,H4ac), C12(H12a,H12b,H12c), C2aa(H2aa,H2ab,H2ac), C19(H19a,H19b,H19c),
 C21(H21a,H21b,H21c), C17(H17a,H17b,H17c), C3aa(H3aa,H3ab,H3ac), C1aa(H1aa,H1ab,
 H1ac), C20(H20a,H20b,H20c)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.907
_oxdiff_exptl_absorpt_empirical_full_min 0.620