Design, structures and study of non-covalent interactions of mono-, di-, and tetranuclear complexes of a bifurcated quadridentate tripod ligand, N-(aminopropyl)-diethanolamine
Sama, Farasha; Ansari, Istikhar A.; Raizada, Mukul; Ahmad, Musheer; Nagaraja, C. M.; Shahid, M.; Kumar, Abhinav; Khan, Kulsum; Siddiqi, Zafar A.; New J. Chem. 41 (2017) 1959–; doi:10.1039/C6NJ02562E

data_7055955
_publ_section_title
;
 Design, structures and study of non-covalent interactions of mono-, di-,
 and tetranuclear complexes of a bifurcated quadridentate tripod ligand,
 N-(aminopropyl)-diethanolamine
;
_journal_issue                   5
_journal_name_full               'New J. Chem.'
_journal_page_first              1959
_journal_paper_doi               10.1039/C6NJ02562E
_journal_volume                  41
_journal_year                    2017
_chemical_formula_moiety
'C14 H34 Cu2 N4 O4, 2(N O3), 1.5(H2 O), 0.5(O)'
_chemical_formula_sum            'C14 H37 Cu2 N6 O12'
_chemical_formula_weight         608.57
_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_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_date             2016-12-29
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_audit_update_record
;
2017-01-16 deposited with the CCDC.
2017-01-17 downloaded from the CCDC.
;
_cell_angle_alpha                76.496(2)
_cell_angle_beta                 84.960(2)
_cell_angle_gamma                60.210(1)
_cell_formula_units_Z            4
_cell_length_a                   11.3213(6)
_cell_length_b                   11.3226(6)
_cell_length_c                   22.7583(12)
_cell_measurement_reflns_used    999
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.50
_cell_measurement_theta_min      2.25
_cell_volume                     2460.4(2)
_computing_cell_refinement       'SAINT 6.45 ( Bruker, 2003)'
_computing_data_collection       'SMART 5.628 (Bruker, 2003)'
_computing_data_reduction        'SAINT 6.45 ( Bruker, 2003)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    SIR-97
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.9990
_diffrn_measured_fraction_theta_max 0.9990
_diffrn_measurement_device_type  'BRUKER SMART APEX'
_diffrn_measurement_method       /w-scans
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0354
_diffrn_reflns_av_unetI/netI     0.0201
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            101107
_diffrn_reflns_theta_full        24.9979
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.24
_exptl_absorpt_coefficient_mu    1.797
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Sadabs
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    1.6428
_exptl_crystal_description       Block
_exptl_crystal_F_000             1271.3595
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.15
_exptl_transmission_factor_max   0.764
_exptl_transmission_factor_min   0.642
_refine_diff_density_max         0.7747
_refine_diff_density_min         -0.4995
_refine_diff_density_rms         0.0740
_refine_ls_d_res_high            0.8409
_refine_ls_d_res_low             9.0881
_refine_ls_goodness_of_fit_ref   1.0562
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    109
_refine_ls_number_parameters     633
_refine_ls_number_reflns         8688
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.0554
_refine_ls_R_factor_all          0.0363
_refine_ls_R_factor_gt           0.0335
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0322P)^2^+4.3948P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0828
_refine_ls_wR_factor_ref         0.0845
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              13
_reflns_limit_k_min              -12
_reflns_limit_l_max              27
_reflns_limit_l_min              0
_reflns_number_gt                8093
_reflns_number_total             8688
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c6nj02562e2.cif
_cod_data_source_block           Complex4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-Scan' changed to
'multi-scan' 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 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 7055955--7055959.cif.
;
_cod_database_code               7055955
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 O2-H2
 0.85 with sigma of 0.01
 O4-H4
 0.85 with sigma of 0.01
 O6-H6
 0.85 with sigma of 0.01
 O8-H8
 0.85 with sigma of 0.01
 C7-H2
 1.893715 with sigma of 0.02
 Cu1-H2
 3.022379 with sigma of 0.02
 C14-H4
 1.88812 with sigma of 0.02
 Cu2-H4
 3.055718 with sigma of 0.02
 C26-H6
 1.888188 with sigma of 0.02
 Cu4-H6
 2.96523 with sigma of 0.02
 C19-H8
 1.888308 with sigma of 0.02
 Cu3-H8
 3.003512 with sigma of 0.02
3.a Free rotating group:
 O1W(H1Wa,H1Wb), O3W(H3Wa,H3Wb), O2W(H2Wa,H2Wb)
3.b Secondary CH2 refined with riding coordinates:
 N2(H2a,H2b), N4(H4a,H4b), C14(H14a,H14b), C13(H13a,H13b), C1(H1a,H1b), C2(H2c,
 H2d), C4(H4c,H4d), C3(H3a,H3b), C6(H6a,H6b), C7(H7a,H7b), C11(H11a,H11b),
 C5(H5a,H5b), C12(H12a,H12b), C10(H10a,H10b), C8(H8a,H8b), C9(H9a,H9b), N6(H6c,
 H6d), N8(H8c,H8d), C20(H20a,H20b), C27(H27a,H27b), C18(H18a,H18b), C19(H19a,
 H19b), C21(H21a,H21b), C25(H25a,H25b), C28(H28a,H28b), C26(H26a,H26b),
 C24(H24a,H24b), C22(H22a,H22b), C23(H23a,H23b), C16(H16a,H16b), C17(H17a,H17b),
  C15(H15a,H15b)
;
_olex2_submission_special_instructions 'No special instructions were received'