Synthesis and Characterization of a Tetrapodal NO4(4-) Ligand and Its Transition Metal Complexes.
Axelson, Jordan C.; Gonzalez, Miguel I.; Meihaus, Katie R.; Chang, Christopher J.; Long, Jeffrey R.; Inorganic chemistry 55 (2016) 7527–7534; doi:10.1021/acs.inorgchem.6b00908

data_4348044
_publ_section_title
;
 Synthesis and Characterization of a Tetrapodal NO4(4-) Ligand and Its
 Transition Metal Complexes.
;
_journal_issue                   15
_journal_name_full               'Inorganic chemistry'
_journal_page_first              7527
_journal_page_last               7534
_journal_paper_doi               10.1021/acs.inorgchem.6b00908
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety
'C13 H11 N O9 Zn, 2(C36 H30 N P2), 24(H2 O)'
_chemical_formula_sum            'C85 H119 N3 O33 P4 Zn'
_chemical_formula_weight         1900.15
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-04-06
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.16 svn.r3265 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                91.799(5)
_cell_angle_beta                 101.041(4)
_cell_angle_gamma                93.168(5)
_cell_formula_units_Z            4
_cell_length_a                   14.7541(10)
_cell_length_b                   23.2242(17)
_cell_length_c                   31.783(2)
_cell_measurement_reflns_used    9897
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.328
_cell_measurement_theta_min      2.432
_cell_volume                     10662.8(13)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker PHOTON100 CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'channel-cut Si(111) crystal'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.8856
_diffrn_reflns_av_R_equivalents  0.0779
_diffrn_reflns_av_unetI/netI     0.0867
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            77147
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        26.410
_diffrn_reflns_theta_max         26.410
_diffrn_reflns_theta_min         2.134
_diffrn_source                   'Advanced Light Source station 11.3.1'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.651
_exptl_absorpt_correction_T_max  0.987
_exptl_absorpt_correction_T_min  0.692
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.1137 before and 0.0758 after correction.
The Ratio of minimum to maximum transmission is 0.7009.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colorless
_exptl_crystal_colour_primary    colorless
_exptl_crystal_density_diffrn    1.155
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3832
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.209
_refine_diff_density_min         -1.241
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2273
_refine_ls_number_reflns         22298
_refine_ls_number_restraints     1806
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.1708
_refine_ls_R_factor_gt           0.1406
_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^)+(0.1146P)^2^+267.6203P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3514
_refine_ls_wR_factor_ref         0.3697
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16189
_reflns_number_total             22298
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            JA019S_sq.cif
_cod_data_source_block           ja019s_sq
_cod_depositor_comments
;

2020-05-08
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C170 H238 N6 O66 P8 Zn2'
_cod_original_formula_weight         3800.30
_cod_original_formula_moiety
'2(C13 H11 N O9 Zn), 4(C36 H30 N P2), 48(H2 O)'
_cod_original_formula_units_Z            2
_cod_original_cell_volume        10662.6(13)
_cod_database_code               4348044
_shelx_estimated_absorpt_t_max   0.987
_shelx_estimated_absorpt_t_min   0.938
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
N6 \\sim P7 \\sim P8: within 2A with sigma of 0.01 and sigma for terminal atoms
of 0.02
C80 \\sim C75 \\sim C76 \\sim C77 \\sim C78 \\sim C79: within 2A with sigma of
0.02 and sigma for terminal atoms of 0.04
3. Rigid body (RIGU) restrains
 Zn1, O4, O9, O2, O6, O1, O8, O3, C6, O7, O5, N1, C11, C3, C7, C1, C2, C4, C10,
  H10, C8, H8, C9, H9, C12, C5, H5A, H5B, H5C, C13, H13A, H13B, H13C
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N2, Zn2, O11, O10, O13, O12, O18, C20, C24, C15, C14, C17, C16, C21, C19, C25,
  C23, O15, O14, O17, O16, H21, C22, C18, C26, H23, H22, H18A, H18B, H18C, H26A,
  H26B, H26C
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C106, N5, P5, C99, C111, C105, P6, C100, C104, C112, C116, C110, C129, C117,
 C123, H100, C101, C103, H104, H112, C113, H116, C115, H106, C107, C109, H110,
 C130, C134, C118, C122, C124, C128, H101, C102, H103, C114, H113, H115, C108,
 H107, H109, C131, H130, H134, C133, H118, C119, C121, H122, H124, C125, H128,
 C127, H102, H114, H108, H131, C132, H133, H119, C120, H121, C126, H125, H127,
 H132, H120, H126
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 P7, P8, N6, C165, C159, C153, C170, C166, C160, C164, C154, C158, C135, C147,
 C141, H170, C169, H166, C167, H160, C161, H164, C163, H154, C155, H158, C157,
 C136, C140, C152, C148, C142, C146, C168, H169, H167, H161, C162, H163, H155,
 C156, H157, H136, C137, H140, C139, H152, C151, H148, C149, C143, H142, H146,
 C145, H168, H162, H156, H137, C138, H139, C150, H151, H149, H143, C144, H145,
 H138, H150, H144
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 P4, P3, N4, C69, C75, C63, C74, C70, C80, C76, C68, C64, C93, C81, C87, H74,
 C73, C71, H70, H80, C79, C77, H76, H68, C67, H64, C65, C98, C94, C86, C82, C88,
  C92, C72, H73, H71, C78, H79, H77, H67, C66, H65, H98, C97, C95, H94, H86,
 C85, H82, C83, C89, H88, C91, H92, H72, H78, H66, H97, C96, H95, H85, C84, H83,
  H89, C90, H91, H96, H84, H90
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C33, P2, N3, C45, C57, C51, P1, C50, C46, C62, C58, C56, C52, C27, C39, H50,
 C49, C47, H46, H62, C61, H58, C59, H56, C55, C53, H52, C28, C32, C34, C38, C44,
  C40, H49, C48, H47, C60, H61, H59, C54, H55, H53, H28, C29, H32, C31, H34,
 C35, H38, C37, H44, C43, C41, H40, H48, H60, H54, H29, C30, H31, C36, H35, H37,
  C42, H43, H41, H30, H36, H42
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Aromatic/amide H refined with riding coordinates:
 C50(H50), C124(H124), C98(H98), C136(H136), C86(H86), C108(H108), C126(H126),
 C152(H152), C100(H100), C109(H109), C54(H54), C170(H170), C72(H72), C101(H101),
  C112(H112), C154(H154), C49(H49), C137(H137), C106(H106), C158(H158),
 C68(H68), C103(H103), C64(H64), C104(H104), C116(H116), C36(H36), C166(H166),
 C131(H131), C130(H130), C62(H62), C82(H82), C110(H110), C125(H125), C34(H34),
 C118(H118), C85(H85), C134(H134), C140(H140), C80(H80), C168(H168), C155(H155),
  C121(H121), C160(H160), C122(H122), C156(H156), C71(H71), C157(H157),
 C74(H74), C56(H56), C139(H139), C73(H73), C58(H58), C161(H161), C143(H143),
 C128(H128), C144(H144), C142(H142), C169(H169), C89(H89), C47(H47), C35(H35),
 C38(H38), C46(H46), C41(H41), C77(H77), C78(H78), C44(H44), C67(H67),
 C107(H107), C138(H138), C37(H37), C53(H53), C83(H83), C132(H132), C114(H114),
 C88(H88), C146(H146), C113(H113), C148(H148), C60(H60), C55(H55), C65(H65),
 C52(H52), C167(H167), C84(H84), C97(H97), C95(H95), C28(H28), C66(H66),
 C32(H32), C119(H119), C76(H76), C150(H150), C164(H164), C149(H149), C145(H145),
  C127(H127), C70(H70), C91(H91), C29(H29), C59(H59), C94(H94), C102(H102),
 C163(H163), C31(H31), C151(H151), C30(H30), C40(H40), C79(H79), C96(H96),
 C48(H48), C120(H120), C133(H133), C42(H42), C115(H115), C92(H92), C61(H61),
 C90(H90), C162(H162), C43(H43), C10(H10), C8(H8), C9(H9), C21(H21), C22(H22),
 C23(H23)
4.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C13(H13A,H13B,H13C), C18(H18A,H18B,H18C), C26(H26A,H26B,H26C)
;
_shelx_res_checksum              94093
_shelx_hkl_checksum              28878
_shelx_fab_checksum              37580
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'