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_4516862
_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 N8 O14 P Zn4, Na, 11.5(H2 O), 3 (H3 O), 3(Cl)'
_chemical_formula_sum            'C62 H90 Cl3 N8 Na O28.5 P Zn4'
_chemical_formula_weight         1825.20
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_audit_creation_date             2016-10-24
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_cell_angle_alpha                90
_cell_angle_beta                 108.074(6)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   32.2177(15)
_cell_length_b                   13.3500(6)
_cell_length_c                   39.051(2)
_cell_measurement_reflns_used    25329
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.627
_cell_measurement_theta_min      3.518
_cell_volume                     15967.3(14)
_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 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0450
_diffrn_reflns_av_unetI/netI     0.0554
_diffrn_reflns_Laue_measured_fraction_full 0.964
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            25329
_diffrn_reflns_point_group_measured_fraction_full 0.964
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         66.627
_diffrn_reflns_theta_min         3.518
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.236
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.519
_exptl_crystal_description       block
_exptl_crystal_F_000             7544
_exptl_crystal_size_max          0.151
_exptl_crystal_size_mid          0.124
_exptl_crystal_size_min          0.099
_refine_diff_density_max         1.142
_refine_diff_density_min         -0.963
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1144
_refine_ls_number_reflns         13918
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.1141
_refine_ls_R_factor_gt           0.0977
_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^)+(0.1872P)^2^+78.3109P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2794
_refine_ls_wR_factor_ref         0.2989
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10940
_reflns_number_total             13918
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao7b00189_si_004.cif
_cod_data_source_block           cluster
_cod_original_cell_volume        15967.3(15)
_cod_original_formula_sum        'C62 H90 Cl3 N8 Na O28.50 P Zn4'
_cod_database_code               4516862
_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(Cl3C) \\sim Ueq, Uanis(Cl3B) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O20) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O28) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Fixed Sof: Zn4(0.75) Zn3(0.75) O6(0.75) H32(0.75) H32A(0.25) O17A(0.5)
 Na1A(0.5) O12(0.75) O13(0.75) Cl2(0.75) O15(0.8) O22(0.6) O18(0.5) Na1(0.5)
 Cl1(0.6) Cl1A(0.4) Cl3(0.5) O28A(0.5) O27A(0.5) Cl3A(0.25) O24A(0.5) O24(0.5)
 Cl2A(0.25) O27(0.5) O18A(0.5) O21A(0.25) O17(0.5) O20(0.5) Zn3A(0.25)
 Zn4A(0.25) O13A(0.25) O12A(0.25) Cl3B(0.125) Cl3C(0.125) O6A(0.25) O15A(0.2)
 O22A(0.4) O28(0.25)
4.a Ternary CH refined with riding coordinates:
 C32(H32), C32(H32A), C1(H1)
4.b Secondary CH2 refined with riding coordinates:
 C34(H34A,H34B), C55(H55A,H55B), C4(H4A,H4B), C3(H3A,H3B), C33(H33A,H33B),
 C2(H2A,H2B), C49(H49A,H49B), C10(H10A,H10B), C35(H35A,H35B), C18(H18A,H18B),
 C41(H41A,H41B), C24(H24A,H24B)
4.c Aromatic/amide H refined with riding coordinates:
 C46(H46), C43(H43), C57(H57), C15(H15), C60(H60), C51(H51), C14(H14),
 C12(H12), C6(H6), C58(H58), C9(H9), C8(H8), C13(H13), C59(H59), C23(H23),
 C52(H52), C44(H44), C7(H7), C26(H26), C28(H28), C29(H29), C20(H20), C27(H27),
 C54(H54), C53(H53), C22(H22), C21(H21), C45(H45), C37(H37), C40(H40), C39(H39),
  C38(H38)
;
_olex2_submission_special_instructions 'No special instructions were received'