Facile C‒H Bond Activation: Synthesis of the N4C Donor Set Pentadentate Ligand 1,4-Bis(2-pyridylmethyl)-1,4-diazacyclononane (dmpdacn) and a Structural Study of Its Alkyl‒Cobalt(III) Complex [Co(dmpdacn-C)(OH2)](ClO4)2·H2O and Its Hydroxylated Derivative [Co(dmpdacnOH-O)Cl](ClO4)2·C3H6O
Zhou, Xiangting; Day, Anthony I.; Edwards, Alison J.; Willis, Anthony C.; Jackson, W. Gregory; Inorganic Chemistry 44 (2005) 452–460; doi:10.1021/ic040081q

data_4308357
_publ_section_title
;
 Facile C--H Bond Activation: Synthesis of the N4C Donor Set Pentadentate
 Ligand 1,4-Bis(2-pyridylmethyl)-1,4-diazacyclononane (dmpdacn) and a
 Structural Study of Its Alkyl--Cobalt(III) Complex
 [Co(dmpdacn-C)(OH2)](ClO4)2&#x00B7;H2O and Its Hydroxylated Derivative
 [Co(dmpdacnOH-O)Cl](ClO4)2&#x00B7;C3H6O
;
_journal_coden_ASTM              INOCAJ
_journal_issue                   2
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              452
_journal_page_last               460
_journal_paper_doi               10.1021/ic040081q
_journal_volume                  44
_journal_year                    2005
_chemical_compound_source        'Local laboratory'
_chemical_formula_moiety         'C19 H26 Cl  Co N4 O,2 Cl O4, C3 H6 O'
_chemical_formula_sum            'C22 H32 Cl3 Co N4 O10'
_chemical_formula_weight         677.840
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             02-02-08
_audit_creation_method           'maXus + CRYSTALS_ver_12-03-99'
_cell_angle_alpha                90.00
_cell_angle_beta                 102.8308(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.78330(10)
_cell_length_b                   11.63720(10)
_cell_length_c                   18.5013(2)
_cell_measurement_reflns_used    50184
_cell_measurement_temperature    200
_cell_measurement_theta_max      30.034
_cell_measurement_theta_min      2.910
_cell_volume                     2683.56(4)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001)'
_computing_data_reduction
'Denzo and Scalepak (Otwinowski & Minor, 1997)'
_computing_molecular_graphics
;
    CAMERON (Watkin et al 1996)
;
_computing_publication_material
;
    CRYSTALS (Watkin et al 2001) + maXus(Mackay et al., 1999)
;
_computing_structure_refinement
;
    CRYSTALS (Watkin et al 2001)
PLATON (Spek 1990)
;
_computing_structure_solution
;
    SIR97 (Altomare et al, 1999)
;
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       KappaCCD
_diffrn_measurement_method       CCD
_diffrn_orient_matrix_type       X=UH
_diffrn_orient_matrix_UB_11      0.07601
_diffrn_orient_matrix_UB_12      -0.02508
_diffrn_orient_matrix_UB_13      -0.00554
_diffrn_orient_matrix_UB_21      -0.02383
_diffrn_orient_matrix_UB_22      -0.05958
_diffrn_orient_matrix_UB_23      -0.05715
_diffrn_orient_matrix_UB_31      0.02031
_diffrn_orient_matrix_UB_32      0.03124
_diffrn_orient_matrix_UB_33      -0.04104
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           ' MoK\a'
_diffrn_radiation_wavelength_id  all
_diffrn_reflns_av_R_equivalents  0.059
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            65043
_diffrn_reflns_theta_full        30.08
_diffrn_reflns_theta_max         30.08
_diffrn_reflns_theta_min         3.03
_exptl_absorpt_coefficient_mu    1.00
_exptl_absorpt_correction_T_max  0.871
_exptl_absorpt_correction_T_min  0.628
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Gaussian integration (Coppens, 1970)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.678
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1400
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.46
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.55
_refine_diff_density_min         -0.44
_refine_diff_density_rms         0.15
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0678
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         3948
_refine_ls_R_factor_gt           0.0413
_refine_ls_shift/su_max          0.000286
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Chebychev polynomial with 3 parameters, Carruthers & Watkin , 1979, 
 17.3    -10.0     12.0    
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0475
_reflns_d_resolution_high        0.60
_reflns_d_resolution_low         1.83
_reflns_number_gt                3948
_reflns_number_total             7860
_reflns_threshold_expression     >3.00\s(I)
_cod_data_source_file            ic040081q_2.cif
_cod_data_source_block           GJXZ3Z
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_atom_sites_solution_hydrogens' value 'geom + difmap' was changed to
'mixed'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_sg_symbol_H-M      'P 21/a '
_cod_original_formula_sum        'C22 H32 Cl3 Co N4 O10 '
_cod_database_code               4308357