Synthesis and characterization of <i>cis</i> and <i>trans</i> cobalt(II) nalidixate complexes having a 1-(4-chlorophenyl)-3-(pyridin-4-ylmethyl)urea ligand.
Brahma, Rinki; Singh, Abhay Pratap; Baruah, Jubaraj Bikash; Dalton transactions (Cambridge, England : 2003) 53 (2024) 14678–14691; doi:10.1039/d4dt01401d

data_7716748
_publ_section_title
;
 Synthesis and characterization of <i>cis</i> and <i>trans</i> cobalt(II)
 nalidixate complexes having a
 1-(4-chlorophenyl)-3-(pyridin-4-ylmethyl)urea ligand.
;
_journal_issue                   35
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14678
_journal_page_last               14691
_journal_paper_doi               10.1039/d4dt01401d
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C50 H46 Cl2 Co N10 O8'
_chemical_formula_sum            'C50 H46 Cl2 Co N10 O8'
_chemical_formula_weight         1044.80
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2023-04-25
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-07-31 deposited with the CCDC.	2024-07-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.540(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.3053(15)
_cell_length_b                   20.015(2)
_cell_length_c                   21.155(2)
_cell_measurement_reflns_used    9961
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      26.08
_cell_measurement_theta_min      2.25
_cell_volume                     5633.4(10)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0380
_diffrn_reflns_av_unetI/netI     0.0199
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            65919
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.925
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.456
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.7024
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0777 before and 0.0551 after correction.
The Ratio of minimum to maximum transmission is 0.9423.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.232
_exptl_crystal_description       block
_exptl_crystal_F_000             2164
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_exptl_transmission_factor_max   0.7454
_exptl_transmission_factor_min   0.7024
_refine_diff_density_max         0.355
_refine_diff_density_min         -0.423
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     323
_refine_ls_number_reflns         4963
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.131
_refine_ls_R_factor_all          0.0825
_refine_ls_R_factor_gt           0.0561
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0868P)^2^+8.0047P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1499
_refine_ls_wR_factor_ref         0.1897
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3622
_reflns_number_total             4963
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01401d2.cif
_cod_data_source_block           rinki2023_0m_a
_cod_depositor_comments
'Adding full bibliography for 7716747--7716749.cif.'
_cod_original_cell_volume        5633.4(11)
_cod_database_code               7716748
_shelx_shelxl_version_number     2019/1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C23(H23A,H23B), C8(H8A,H8B)
2.b Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), C11(H11), C16(H16), C20(H20), C10(H10), C12(H12), C19(H19),
 C13(H13), C3(H3), C2(H2A), C5(H5), C6(H6)
2.c Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C24(H24A,H24B,H24C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 260 electrons were 
found in a volume of 1212\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
0.077[C3H7NO], 0.154[H2O] per Asymmetric Unit 
which account for 240 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              29029
_shelx_hkl_checksum              5524
_shelx_fab_checksum              14029
_olex2_submission_special_instructions 'No special instructions were received'