An investigation of 1,4,7-tri(4-alkynyl)-1,4,7-triazacyclononanes: ligand synthesis and metal co-ordination chemistry †
Baker, Murray V.; Brown, David H.; Skelton, Brian W.; White, Allan H.; Journal of the Chemical Society, Dalton Transactions  (2000) 4607–; doi:10.1039/b007324p

data_7010246
_publ_section_title
;
 An investigation of 1,4,7-tri(4-alkynyl)-1,4,7-triazacyclononanes:
 ligand synthesis and metal co-ordination chemistry&#x200A;&#x2020;
;
_journal_issue                   24
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              4607
_journal_paper_doi               10.1039/b007324p
_journal_year                    2000
_chemical_formula_sum            'C45 H51 Mo N3 O4'
_chemical_formula_weight         793.86
_space_group_IT_number           45
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'I 2 -2c'
_symmetry_space_group_name_H-M   'I b a 2'
_cell_angle_alpha                90.00000
_cell_angle_beta                 90.00000
_cell_angle_gamma                90.00000
_cell_formula_units_Z            8
_cell_length_a                   25.283(5)
_cell_length_b                   14.986(3)
_cell_length_c                   21.337(4)
_cell_measurement_reflns_used    7736
_cell_measurement_temperature    153
_cell_measurement_theta_max      28
_cell_measurement_theta_min      2
_cell_volume                     8084(3)
_computing_cell_refinement       'Siemens SAINT (Siemens, 1995)'
_computing_data_collection       'Siemens SMART (Siemens, 1995)'
_computing_data_reduction        'xtal ADDREF SORTRF'
_computing_molecular_graphics    xtal
_computing_publication_material  'xtal BONDLA CIFIO'
_computing_structure_refinement  'xtal CRYLSQ'
_computing_structure_solution    xtal
_diffrn_ambient_temperature      153
_diffrn_measurement_device_type
;
Bruker SMART CCD diffractometer
;
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_detector       'CCD area detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .048
_diffrn_reflns_av_sigmaI/netI    .05
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       20
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_diffrn_reflns_limit_l_min       -28
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_diffrn_reflns_theta_max         29.17
_diffrn_reflns_theta_min         1.91
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    .37
_exptl_absorpt_correction_T_max  .901
_exptl_absorpt_correction_T_min  .824
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS, Sheldrick, 1996
;
_exptl_crystal_density_diffrn    1.304
_exptl_crystal_description       prism
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_exptl_crystal_size_mid          .3
_exptl_crystal_size_min          .15
_refine_diff_density_max         1.099
_refine_diff_density_min         -.705
_refine_ls_abs_structure_details 'Flack xabs refined'
_refine_ls_abs_structure_Flack   -.02(5)
_refine_ls_goodness_of_fit_all   1.485
_refine_ls_goodness_of_fit_ref   1.548
_refine_ls_hydrogen_treatment    noref
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_refine_ls_R_factor_all          .051
_refine_ls_R_factor_gt           .037
_refine_ls_shift/su_max          .05
_refine_ls_shift/su_mean         .004
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         .049
_refine_ls_wR_factor_ref         .045
_reflns_d_resolution_high        .729
_reflns_d_resolution_low         10.646
_reflns_Friedel_coverage         .968
_reflns_limit_h_max              34
_reflns_limit_h_min              0
_reflns_limit_k_max              20
_reflns_limit_k_min              0
_reflns_limit_l_max              29
_reflns_limit_l_min              0
_reflns_number_gt                5249
_reflns_number_total             5249
_reflns_threshold_expression     'F    > 4.00 sig(F   )'
_cod_data_source_file            b007324p.txt
_cod_data_source_block           dbmol
_cod_original_sg_symbol_Hall     i_2_-2c
_cod_original_sg_symbol_H-M      I_b_a_2
_cod_original_formula_sum        'C45 H51 Mo1 N3 O4'
_cod_database_code               7010246