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_7221819
_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 Cd N8 O10'
_chemical_formula_sum            'C22 H22 Cd N8 O10'
_chemical_formula_weight         670.88
_chemical_name_systematic
;
diaquadi(N-4-pyridylnicotinamide)cadmium(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   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-10-02
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_audit_update_record
;
2015-08-05 deposited with the CCDC.
2015-08-18 downloaded from the CCDC.
;
_cell_angle_alpha                76.1428(18)
_cell_angle_beta                 73.5323(18)
_cell_angle_gamma                83.610(2)
_cell_formula_units_Z            1
_cell_length_a                   7.3668(5)
_cell_length_b                   9.1365(6)
_cell_length_c                   9.9565(6)
_cell_measurement_reflns_used    9875
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      31.54
_cell_measurement_theta_min      2.30
_cell_volume                     623.27(7)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 v.2013.4_1 (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (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., 2013)'
_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  D8Venture
_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  0.0651
_diffrn_reflns_av_unetI/netI     0.0388
_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            19999
_diffrn_reflns_theta_full        29.00
_diffrn_reflns_theta_max         29.00
_diffrn_reflns_theta_min         2.30
_diffrn_source                   'ImuS microsource'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.951
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7122
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1382 before and 0.1127 after correction.
The Ratio of minimum to maximum transmission is 0.7122.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'dull dark colourless'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.787
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             338
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.902
_refine_diff_density_min         -1.292
_refine_diff_density_rms         0.297
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     157
_refine_ls_number_reflns         3310
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.0595
_refine_ls_R_factor_gt           0.0592
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1200P)^2^+0.7000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1492
_refine_ls_wR_factor_ref         0.1497
_reflns_number_gt                3264
_reflns_number_total             3310
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ce00901d2.cif
_cod_data_source_block           Complex4
_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               7221819
_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, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O5-H5A \\sim O5-H5B
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
Uiso(C7B) = Uiso(C7A)
4. Others
 Fixed Sof: C7A(0.5) C11A(0.5) H11A(0.5) C10A(0.5) H10A(0.5) C9A(0.5) H9A(0.5)
 N3A(0.5) C8A(0.5) H8A(0.5) C7B(0.5) C11B(0.5) H11B(0.5) N3B(0.5) C10B(0.5)
 H10B(0.5) C9B(0.5) H9B(0.5) C8B(0.5) H8B(0.5)
5.a Rotating group:
 O5(H5A,H5B)
5.b Aromatic/amide H refined with riding coordinates:
 N2(H2), C1(H1), C2(H2A), C4(H4), C5(H5), C11A(H11A), C10A(H10A), C9A(H9A),
 C8A(H8A), C11B(H11B), C10B(H10B), C9B(H9B), C8B(H8B)
5.c Fitted hexagon refined as free rotating group:
 C7A(C11A,C10A,C9A,N3A,C8A), C7B(C11B,N3B,C10B,C9B,C8B)
;
_olex2_submission_special_instructions 'No special instructions were received'