Inorganic Phosphate and Arsenate within New Tetranuclear Copper and Zinc Complexes: Syntheses, Crystal Structures, Magnetic, Electrochemical, and Thermal Studies.
Haldar, Shobhraj; Vijaykumar, Gonela; Carrella, Luca; Batha, Steven; Musie, Ghezai T.; Bera, Manindranath; ACS omega 2 (2017) 1535–1549; doi:10.1021/acsomega.7b00189

data_4516860
_publ_section_title
;
 Inorganic Phosphate and Arsenate within New Tetranuclear Copper and Zinc
 Complexes: Syntheses, Crystal Structures, Magnetic, Electrochemical, and
 Thermal Studies.
;
_journal_issue                   4
_journal_name_full               'ACS omega'
_journal_page_first              1535
_journal_page_last               1549
_journal_paper_doi               10.1021/acsomega.7b00189
_journal_volume                  2
_journal_year                    2017
_chemical_formula_moiety
'C62 H58 Cu4 N8 O14 P, 3 Na, 14 (H2 O), 2 (H O)'
_chemical_formula_sum            'C62 H88 Cu4 N8 Na3 O30 P'
_chemical_formula_weight         1779.50
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-01-25
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.9275(11)
_cell_length_b                   10.7050(4)
_cell_length_c                   30.4859(10)
_cell_measurement_reflns_used    6578
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      27.4410
_cell_measurement_theta_min      1.7810
_cell_volume                     7482.4(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33c (release 11-04-2014 CrysAlis171 .NET)
(compiled Apr 11 2014,15:12:41)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33c (release 11-04-2014 CrysAlis171 .NET)
(compiled Apr 11 2014,15:12:41)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33c (release 11-04-2014 CrysAlis171 .NET)
(compiled Apr 11 2014,15:12:41)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution
;
olex2.solve (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9580
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.892
_diffrn_measurement_details
;
  1 omega  -11.00   53.00   1.0000  210.2900
omega____ theta____ kappa____ phi______ frames
    -       27.3512   57.0000   60.0000 64

  2 omega  -45.00   71.00   1.0000  210.2900
omega____ theta____ kappa____ phi______ frames
    -       27.3512  -38.0000 -180.0000 116
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0111848000
_diffrn_orient_matrix_UB_12      -0.0275747000
_diffrn_orient_matrix_UB_13      0.0194054000
_diffrn_orient_matrix_UB_21      -0.0255293000
_diffrn_orient_matrix_UB_22      -0.0370525000
_diffrn_orient_matrix_UB_23      0.0017959000
_diffrn_orient_matrix_UB_31      0.0134483000
_diffrn_orient_matrix_UB_32      -0.0475140000
_diffrn_orient_matrix_UB_33      -0.0126926000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0360
_diffrn_reflns_av_unetI/netI     0.0554
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.892
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            19460
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.892
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.161
_diffrn_reflns_theta_min         1.604
_exptl_absorpt_coefficient_mu    1.250
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.51017
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33c (release 11-04-2014 CrysAlis171 .NET)
(compiled Apr 11 2014,15:12:41)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.580
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3680
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.24
_refine_diff_density_max         1.353
_refine_diff_density_min         -0.976
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     533
_refine_ls_number_reflns         8197
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.1093
_refine_ls_R_factor_gt           0.0722
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0711P)^2^+48.9370P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1750
_refine_ls_wR_factor_ref         0.1977
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5687
_reflns_number_total             8197
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao7b00189_si_002.cif
_cod_data_source_block           cluster
_cod_database_code               4516860
_shelxl_version_number           2012-9
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O9) \\sim Ueq, Uanis(O14A) \\sim Ueq, Uanis(O10A) \\sim Ueq, Uanis(O14)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Fixed Sof: O12(0.75) O13(0.6) O10(0.6) O10A(0.4) O12A(0.25) O14(0.6) O15(0.6)
 O15A(0.4) O13A(0.4) O14A(0.4)
4.a Ternary CH refined with riding coordinates:
 C1(H1)
4.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C12(H12A,H12B), C18(H18A,H18B),
 C26(H26A,H26B)
4.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C9(H9), C14(H14), C15(H15), C16(H16), C17(H17),
 C20(H20), C21(H21), C22(H22), C23(H23), C28(H28), C29(H29), C30(H30), C31(H31)
;
_shelx_res_checksum              49068
_shelx_hkl_checksum              98263
_olex2_submission_special_instructions 'No special instructions were received'