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_4516861
_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 As Cu4 N8 O14), 2(K), (H O), 16.67 (H2 O)'
_chemical_formula_sum            'C62 H92.3 As Cu4 K2 N8 O31.67'
_chemical_formula_weight         1863.73
_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             2016-11-23
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.07 svn.r3352 for OlexSys, GUI svn.r5261)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.4332(6)
_cell_length_b                   10.3864(3)
_cell_length_c                   30.7434(9)
_cell_measurement_reflns_used    11976
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      26.4320
_cell_measurement_theta_min      2.1550
_cell_volume                     7482.5(4)
_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
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_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 0.995
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
  1 omega  -10.00   99.50   0.7500   90.3700
omega____ theta____ kappa____ phi______ frames
    -       27.6637   77.0000  120.0000 146

  2 omega   22.00  103.00   0.7500   90.3700
omega____ theta____ kappa____ phi______ frames
    -       27.6637   57.0000  -90.0000 108

  3 omega   39.00  118.50   0.7500   90.3700
omega____ theta____ kappa____ phi______ frames
    -       27.6637  178.0000   90.0000 106
;
_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      0.0161829000
_diffrn_orient_matrix_UB_12      -0.0380326000
_diffrn_orient_matrix_UB_13      -0.0146601000
_diffrn_orient_matrix_UB_21      -0.0025217000
_diffrn_orient_matrix_UB_22      0.0487629000
_diffrn_orient_matrix_UB_23      -0.0160293000
_diffrn_orient_matrix_UB_31      0.0254639000
_diffrn_orient_matrix_UB_32      0.0289983000
_diffrn_orient_matrix_UB_33      0.0077446000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0266
_diffrn_reflns_av_unetI/netI     0.0248
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            28453
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         1.738
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.764
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64993
_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            'clear bluish blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   bluish
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.654
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3843
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.926
_refine_diff_density_min         -0.629
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     578
_refine_ls_number_reflns         7610
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0538
_refine_ls_R_factor_gt           0.0479
_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^)+(0.0675P)^2^+17.1967P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1321
_refine_ls_wR_factor_ref         0.1364
_reflns_number_gt                6826
_reflns_number_total             7610
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao7b00189_si_003.cif
_cod_data_source_block           cluster
_cod_original_cell_volume        7482.5(3)
_cod_original_formula_sum        'C62 H92.30 As Cu4 K2 N8 O31.67'
_cod_database_code               4516861
_shelxl_version_number           2012-9
_reflns_odcompleteness_completeness 99.18
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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(O11B) \\sim Ueq, Uanis(O12B) \\sim Ueq, Uanis(O12) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Fixed Sof: K1(0.65) O15(0.65) K1B(0.35) O15B(0.35) O9(0.65) O11(0.65)
 O9B(0.35) O11B(0.35) O12(0.65) O12B(0.175) O14(0.65) O14B(0.35) O13(0.65)
 O13B(0.35) O8(0.65) O8B(0.35) O16(0.34) O16B(0.33) O16A(0.34)
4.a Ternary CH refined with riding coordinates:
 C1(H1)
4.b Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C4(H4A,H4B), C2(H2A,H2B), C3(H3A,H3B), C18(H18A,H18B),
 C26(H26A,H26B)
4.c Aromatic/amide H refined with riding coordinates:
 C17(H17), C16(H16), C15(H15), C14(H14), C6(H6), C7(H7), C8(H8), C9(H9),
 C20(H20), C21(H21), C22(H22), C23(H23), C31(H31), C30(H30), C29(H29), C28(H28)
;
_olex2_submission_special_instructions 'No special instructions were received'