Synthesis and structure of mononuclear and binuclear zinc(ii) compartmental macrocyclic complexes
Atkins, Andrew J.; Black, Daniel; Finn, Rachel L.; Marin-Becerra, Armando; Blake, Alexander J.; Ruiz-Ramirez, Lena; Li, Wan-Sheung; Schröder, Martin; Dalton Transactions  (2003) 1730–; doi:10.1039/b210936k

data_7012434
_publ_section_title
;
 Synthesis and structure of mononuclear and binuclear zinc(ii)
 compartmental macrocyclic complexes
;
_journal_issue                   9
_journal_name_full               'Dalton Transactions'
_journal_page_first              1730
_journal_paper_doi               10.1039/b210936k
_journal_year                    2003
_chemical_formula_moiety         'C26 H29 N4 O4 P Zn2 +, P F6 -, C2 H3 N'
_chemical_formula_sum            'C28 H32 F6 N5 O4 P Zn2'
_chemical_formula_weight         778.30
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   'difference Fourier; geometrically placed'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.85(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.736(4)
_cell_length_b                   12.177(5)
_cell_length_c                   16.237(4)
_cell_measurement_reflns_used    26
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      16.3
_cell_measurement_theta_min      12.65
_cell_volume                     3074.2(17)
_computing_cell_refinement       STADI-4
_computing_data_collection       'STADI-4 (Stoe, 1995)'
_computing_data_reduction        'X-RED (Stoe, 1995)'
_computing_molecular_graphics    'SHELXTL/PC (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97; PLATON (Spek, 2002)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.950
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_device_type  'Stoe Stadi-4'
_diffrn_measurement_method       Omega-theta
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.021
_diffrn_reflns_av_sigmaI/netI    0.034
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -2
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            7222
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.0
_diffrn_reflns_theta_min         2.54
_diffrn_standards_decay_%        'random variation +- 2.05'
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.693
_exptl_absorpt_correction_T_max  0.958
_exptl_absorpt_correction_T_min  0.727
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            'thick plate'
_exptl_crystal_density_diffrn    1.682
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       orange
_exptl_crystal_F_000             1584
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.67
_refine_diff_density_min         -0.47
_refine_diff_density_rms         0.09
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.171
_refine_ls_hydrogen_treatment    'rigid rotating group; riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     436
_refine_ls_number_reflns         5411
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      1.169
_refine_ls_R_factor_all          0.0659
_refine_ls_R_factor_gt           0.0464
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.018P)^2^+10.11P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0868
_refine_ls_wR_factor_ref         0.101
_reflns_number_gt                4401
_reflns_number_total             5411
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b210936k.txt
_cod_data_source_block           5
_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:

'_exptl_absorpt_correction_type' tag value 'psi-scans' was replaced
with 'psi-scan' value.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.018P)^2^+10.11P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.018P)^2^+10.11P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7012434