Selective gelation of N-(4-pyridyl)nicotinamide by copper(ii) salts
Ghosh, Dipankar; Lebedytė, Ieva; Yufit, Dmitry S.; Damodaran, Krishna K.; Steed, Jonathan W.; CrystEngComm 17 (2015) 8130–; doi:10.1039/C5CE00901D

data_7221817
_publ_section_title
;
 Selective gelation of N-(4-pyridyl)nicotinamide by copper(ii) salts
;
_journal_issue                   42
_journal_name_full               CrystEngComm
_journal_page_first              8130
_journal_paper_doi               10.1039/C5CE00901D
_journal_volume                  17
_journal_year                    2015
_chemical_formula_moiety         'C22 H22 N8 O10 Zn'
_chemical_formula_sum            'C22 H22 N8 O10 Zn'
_chemical_formula_weight         623.85
_chemical_name_systematic
;
diaquadi(N-4-pyridylnicotinamide)zinc(II)nitrate 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-04-29
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-08-05 deposited with the CCDC.
2015-08-18 downloaded from the CCDC.
;
_cell_angle_alpha                75.2719(17)
_cell_angle_beta                 72.7974(17)
_cell_angle_gamma                82.7345(17)
_cell_formula_units_Z            1
_cell_length_a                   7.4378(4)
_cell_length_b                   8.9941(4)
_cell_length_c                   9.8914(5)
_cell_measurement_reflns_used    6917
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      31.40
_cell_measurement_theta_min      2.21
_cell_volume                     610.39(5)
_computing_cell_refinement       'APEX2 v.2013.4_1 (Bruker, 2013)'
_computing_data_collection       'APEX2 v.2013.4_1 (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.30C (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      120.0
_diffrn_detector                 'Bruker PHOTON 100 CMOS'
_diffrn_detector_type            'CMOS sensor'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'Bruker D8 Venture'
_diffrn_measurement_device_type  '3-circle diffractometer'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_monochromator  'focusing mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0358
_diffrn_reflns_av_unetI/netI     0.0387
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            13125
_diffrn_reflns_theta_full        29.50
_diffrn_reflns_theta_max         29.50
_diffrn_reflns_theta_min         2.21
_diffrn_source                   'ImuS microsource'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.083
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9298
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.0615 before and 0.0468 after correction.
The Ratio of minimum to maximum transmission is 0.9298.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.697
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             320
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.015
_refine_diff_density_max         0.384
_refine_diff_density_min         -0.326
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         3403
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_gt           0.0343
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+0.4500P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0736
_refine_ls_wR_factor_ref         0.0777
_reflns_number_gt                2891
_reflns_number_total             3403
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ce00901d2.cif
_cod_data_source_block           Complex3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according
to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 7221817--7221820.cif.
;
_cod_database_code               7221817
_computing.bruker_data_scaling   'SADABS V2012/1 (Bruker AXS Inc.)'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Shared sites
{C4B, N3B}
{C4A, N3A}
3. Uiso/Uaniso restraints and constraints
Uanis(C4A) = Uanis(N3A)
Uanis(C4B) = Uanis(N3B)
4. Others
 Fixed Sof: N3A(0.5) N3B(0.5) C4A(0.5) H4A(0.5) C4B(0.5) H4B(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4A(H4A), C4B(H4B), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11)
;
_olex2_submission_special_instructions 'No special instructions were received'