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_4308356
_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_formula_moiety         ' C19 H27 Co N4 O 2+, 2(Cl O4 -), H2 O'
_chemical_formula_sum            'C19 H29 Cl2 Co N4 O10'
_chemical_formula_weight         603.30
_chemical_melting_point          ?
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             03-30-10
_audit_creation_method           CRYSTALS_ver_12-03-99
_audit_update_record
;
Report for 
wgj2
C19 H29 Cl2 Co N4 O10
W. Greg Jackson and Xiangting Zhou, ADFA
2000-05-01  acw finishes refinement and compiles cif
2000-05-02  passes checkcif with minor alerts 
2003-10-29  re-refined in CRYSTALS, relabelled, cif for publication
;
_cell_angle_alpha                90
_cell_angle_beta                 108.4631(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.1169(2)
_cell_length_b                   25.5635(6)
_cell_length_c                   11.4461(2)
_cell_measurement_reflns_used    18207
_cell_measurement_temperature    295
_cell_measurement_theta_max      27
_cell_measurement_theta_min      3
_cell_volume                     2530.32(9)
_computing_cell_refinement
; 
 Denzo/Scalepack (Otwinowski & Minor, 1996) 
;
_computing_data_collection
; 
 COLLECT (Nonius BV, 1997) 
;
_computing_data_reduction
; 
 Denzo/Scalepack (Otwinowski & Minor, 1996) 
;
_computing_molecular_graphics
; 
ORTEP-II (Johnson 1976) in teXsan (MSC, 1992-1997)
;
_computing_publication_material
; 
 CRYSTALS (Watkin et al 2001) 
;
_computing_structure_refinement
; 
 CRYSTALS (Watkin et al 2001) 
;
_computing_structure_solution
; 
 SIR92 (Altomare et al, 1994) 
;
_diffrn_ambient_temperature      295
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type
; 
Enraf Nonius Kappa CCD 
;
_diffrn_measurement_method       ' \f and \w scans with CCD '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.034
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            26780
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         4.08
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.949
_exptl_absorpt_correction_T_max  .850
_exptl_absorpt_correction_T_min  .751
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;
_exptl_crystal_colour            ' orange '
_exptl_crystal_density_diffrn    1.584
_exptl_crystal_density_meas      ?
_exptl_crystal_description       ' block '
_exptl_crystal_F_000             1248.00
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.50
_refine_diff_density_min         -0.54
_refine_ls_abs_structure_details 'Flack, 2692 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.350(13)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0378
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     349
_refine_ls_number_reflns         4592
_refine_ls_R_factor_gt           0.0323
_refine_ls_shift/su_max          0.002408
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Chebychev polynomial with 3 parameters, Carruthers & Watkin , 1979, 
0.597    0.340    0.254    
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0386
_reflns_limit_h_max              11
_reflns_limit_h_min              -11
_reflns_limit_k_max              33
_reflns_limit_k_min              0
_reflns_limit_l_max              14
_reflns_limit_l_min              -14
_reflns_number_gt                4592
_reflns_number_total             5598
_reflns_threshold_expression     >3.00\s(I)
_cod_data_source_file            ic040081q_1.cif
_cod_data_source_block           wgj2new2
_cod_depositor_comments
;
 Homogenising atom type symbols in order to relate data from different loops.

 Antanas Vaitkus,
 2017-03-04

The following automatic conversions were performed:
_chemical_melting_point value 'not measured' changed to '?' - value
is undefined or not given.
Automatic conversion script
Id: cif_fix_values 1382 2010-08-28 14:56:29Z saulius 

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:
data name '_geom_bond_atom_site_label_D' replaced with
'_geom_hbond_atom_site_label_D' as specified in the replacement file
'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_tags.lst'.

data
name '_geom_bond_atom_site_label_H' replaced with
'_geom_hbond_atom_site_label_H' as specified in the replacement file
'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_tags.lst'.

data
name '_geom_contact_atom_site_label_a' replaced with
'_geom_hbond_atom_site_label_A' as specified in the replacement file
'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_tags.lst'.

data
name '_geom_bond_distance_DH' replaced with '_geom_hbond_distance_DH'
as specified in the replacement file
'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_tags.lst'.

data
name '_geom_contact_distance_HA' replaced with
'_geom_hbond_distance_HA' as specified in the replacement file
'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_tags.lst'.

data
name '_geom_contact_distance_DA' replaced with
'_geom_hbond_distance_DA' as specified in the replacement file
'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_tags.lst'.

data
name '_geom_angle_DHA' replaced with '_geom_hbond_angle_DHA' as
specified in the replacement file
'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_tags.lst'.

data
name '_geom_contact_site_symmetry_A' replaced with
'_geom_hbond_site_symmetry_A' as specified in the replacement file
'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 5005 2017-03-03 11:38:54Z antanas 
;
_cod_original_sg_symbol_H-M      'C 1 c 1 '
_cod_original_formula_sum        ' C19 H29 Cl2 Co N4 O10 '
_cod_database_code               4308356