Hydrolytically active tetranuclear [NiII2]2 complexes: synthesis, structure, spectroscopy and phosphoester hydrolysis
Giri, Gopal C.; Patra, Ayan; Vijaykumar, Gonela; Carrella, Luca; Bera, Manindranath; RSC Advances 5 (2015) 99270–; doi:10.1039/C5RA16555E

data_7235970
_publ_section_title
;
 Hydrolytically active tetranuclear [NiII2]2 complexes: synthesis,
 structure, spectroscopy and phosphoester hydrolysis
;
_journal_issue                   120
_journal_name_full               'RSC Advances'
_journal_page_first              99270
_journal_paper_doi               10.1039/C5RA16555E
_journal_volume                  5
_journal_year                    2015
_chemical_formula_moiety
'C46 H62 N4 Ni4 O18, 3.2(C H4 O), 2(Cl O4), 0.8(O)'
_chemical_formula_sum            'C49.2 H76.4 Cl2 N4 Ni4 O30'
_chemical_formula_weight         1509.62
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2015-07-31
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-11-09 deposited with the CCDC.
2015-11-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.6138(3)
_cell_length_b                   17.4519(3)
_cell_length_c                   19.6556(5)
_cell_measurement_temperature    293(2)
_cell_volume                     6042.0(2)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'SIR-97/(Altomare, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'OMEGA-PHI SCAN'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0317
_diffrn_reflns_av_unetI/netI     0.0345
_diffrn_reflns_Laue_measured_fraction_full 0.920
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            14044
_diffrn_reflns_point_group_measured_fraction_full 0.920
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         66.198
_diffrn_reflns_theta_min         5.022
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.037
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'BRUKER SADABS'
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.670
_exptl_crystal_description       Block
_exptl_crystal_F_000             3160
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.13
_exptl_transmission_factor_max   0.674
_exptl_transmission_factor_min   0.545
_refine_diff_density_max         1.900
_refine_diff_density_min         -0.642
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     417
_refine_ls_number_reflns         5032
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0637
_refine_ls_R_factor_gt           0.0587
_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^)+(0.0917P)^2^+18.7980P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1609
_refine_ls_wR_factor_ref         0.1673
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4536
_reflns_number_total             5032
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ra16555e2.cif
_cod_data_source_block           complex
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'MULTI-SCAN' was
changed to 'multi-scan' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_database_code               7235970
_shelxl_version_number           2012-9
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H18 of O18, H23 of O23, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, H1 of O1, H39 of O39, All O(H,H) groups
2. Others
 Fixed Sof: O1(0.6) H1(0.6) C1(0.6) H1A(0.6) H1B(0.6) H1C(0.6) O50B(0.4)
3.a Riding coordinates:
 O1(H1), O18(H18), O23(H23), O36(H36A,H36B), O37(H37A,H37B), O39(H39)
3.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C12(H12A,H12B), C14(H14A,H14B), C16(H16A,H16B), C17(H17A,
 H17B), C19(H19A,H19B), C21(H21A,H21B), C22(H22A,H22B)
3.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C8(H8), C29(H29), C30(H30), C31(H31), C32(H32)
3.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C40(H40A,H40B,H40C)
;
_shelx_res_checksum              82521
_olex2_submission_special_instructions 'No special instructions were received'