New topologies in pentanuclear nickel/oximato clusters: structural and magnetic characterization.
Esteban, Jordi; Font-Bardia, Mercè; Costa, José Sánchez; Teat, Simon J.; Escuer, Albert; Inorganic chemistry 53 (2014) 3194–3203; doi:10.1021/ic500057j

data_4337613
_publ_section_title
;
 New topologies in pentanuclear nickel/oximato clusters: structural and
 magnetic characterization.
;
_journal_issue                   6
_journal_name_full               'Inorganic chemistry'
_journal_page_first              3194
_journal_page_last               3203
_journal_paper_doi               10.1021/ic500057j
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety
'C98 H75 N12 Ni5 O17, C8 H20 N, 3(CH2Cl2), H2O'
_chemical_formula_sum            'C109 H102 Cl6 N13 Ni5 O18'
_chemical_formula_weight         2388.19
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-01-31
_audit_creation_method
;
  Olex2 1.2
  (compiled Dec  5 2012 16:20:19, GUI svn.r4385)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 112.758(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.7339(18)
_cell_length_b                   24.440(3)
_cell_length_c                   28.002(3)
_cell_measurement_reflns_used    6675
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.9785
_cell_measurement_theta_min      2.9965
_cell_volume                     10561(2)
_computing_cell_refinement       'Bruker SAINT v7.56a'
_computing_data_collection       'Bruker APEX 2'
_computing_data_reduction        'Bruker SAINT v7.56a'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  '\w rotation with narrow frames'
_diffrn_radiation_monochromator  'Bruker APEX II CCD diffractometer'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.77490
_diffrn_reflns_av_R_equivalents  0.0733
_diffrn_reflns_av_unetI/netI     0.0526
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            41911
_diffrn_reflns_theta_full        20.82
_diffrn_reflns_theta_max         20.82
_diffrn_reflns_theta_min         2.87
_diffrn_source                   'Advanced Light Source station 11.3.1'
_exptl_absorpt_coefficient_mu    1.374
_exptl_absorpt_correction_T_max  0.74
_exptl_absorpt_correction_T_min  0.60
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2.10 Bruker AXS Madison WI US'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.502
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4931
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.749
_refine_diff_density_min         -0.697
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1354
_refine_ls_number_reflns         8501
_refine_ls_number_restraints     55
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.1081
_refine_ls_R_factor_gt           0.0725
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1306P)^2^+37.3646P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1940
_refine_ls_wR_factor_ref         0.2217
_reflns_number_gt                5654
_reflns_number_total             8501
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic500057j_si_001.cif
_cod_data_source_block           je280
_cod_database_code               4337613
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H6(0.086) H13B(0.127) H4(0.088) H1(0.096) H52(0.108) H2(0.107)
 H8(0.103) H3(0.098) H32(0.109) H4A(0.087) H36(0.131) H33(0.137) H34(0.165)
 H35(0.169) H30(0.08) H9(0.107) H10(0.1) H11(0.094) H15(0.083) H16(0.096)
 H17(0.095) H18(0.087) H22(0.083) H23(0.089) H24(0.096) H25(0.096) H38(0.099)
 H5A(0.151) H0A(0.192) H2A(0.238) H3A(0.245) H4AA(0.17) H29(0.083) H40(0.15)
 H41(0.091) H0B(0.106) H39(0.107) H8A(0.107) H7A(0.1) H84(0.082) H83(0.103)
 H82(0.089) H81(0.095) H80(0.092) H72(0.086) H78(0.104) H77(0.121) H76(0.125)
 H75(0.127) H74(0.104) H1B(0.137) H66(0.092) H67(0.117) H68(0.141) H69(0.131)
 H3B(0.117) H70(0.11) H58(0.085) H2B(0.129) H60(0.103) H61(0.125) H62(0.151)
 H63(0.192) H64(0.152) H46(0.115) H47(0.137) H48(0.143) H49(0.153) H50(0.136)
 H56(0.116) H55(0.168) H54(0.151) H53(0.126) H44(0.087) H91A(0.128) H91B(0.128)
 H92A(0.069) H92B(0.069) H92C(0.069) H87A(0.137) H87B(0.137) H88A(0.162)
 H88B(0.162) H88C(0.162) H86A(0.15) H86B(0.15) H85A(0.114) H85B(0.114)
 H85C(0.114) H90A(0.133) H90B(0.133) H89A(0.078) H89B(0.078) H89C(0.078)
 Fixed X: H6(0.2568) H13B(0.2413) H4(0.2519) H1(0.2227) H52(0.0365) H2(0.1464)
 H8(0.2054) H3(-0.0023) H32(0.0091) H4A(-0.0698) H36(0.1773) H33(-0.0386)
 H34(0.0173) H35(0.1223) H30(0.1751) H9(0.1241) H10(-0.0248) H11(-0.0857)
 H15(0.4578) H16(0.5097) H17(0.4372) H18(0.3081) H22(0.4604) H23(0.5182)
 H24(0.4464) H25(0.3192) H38(-0.0327) H5A(0.3525) H0A(0.318) H2A(0.3695)
 H3A(0.4556) H4AA(0.49) H29(0.4778) H40(-0.1051) H41(0.4518) H0B(0.5674)
 H39(0.7067) H8A(0.7371) H7A(0.6221) H84(0.5668) H83(0.6475) H82(0.6993)
 H81(0.6723) H80(0.5906) H72(0.5173) H78(0.6127) H77(0.6881) H76(0.6784)
 H75(0.6003) H74(0.5319) H1B(0.0285) H66(0.4473) H67(0.5648) H68(0.7052)
 H69(0.7272) H3B(0.1258) H70(0.6101) H58(0.4614) H2B(-0.1335) H60(0.3412)
 H61(0.3048) H62(0.3497) H63(0.4304) H64(0.4716) H46(0.3433) H47(0.4709)
 H48(0.4709) H49(0.3408) H50(0.216) H56(0.2571) H55(0.208) H54(0.0836) H53(-
 0.0063) H44(0.1329) H91A(-0.2098) H91B(-0.1722) H92A(-0.1057) H92B(-0.0308)
 H92C(-0.0889) H87A(-0.024) H87B(-0.0008) H88A(-0.0906) H88B(-0.0898) H88C(-
 0.001) H86A(-0.045) H86B(-0.0756) H85A(-0.1881) H85B(-0.1457) H85C(-0.2186)
 H90A(-0.2232) H90B(-0.2468) H89A(-0.2275) H89B(-0.1634) H89C(-0.1276)
 Fixed Y: H6(-0.1812) H13B(-0.3377) H4(-0.2884) H1(0.0243) H52(-0.1175)
 H2(0.1023) H8(-0.4822) H3(0.0938) H32(-0.1672) H4A(0.0105) H36(-0.1871) H33(-
 0.0883) H34(-0.0578) H35(-0.1075) H30(-0.2523) H9(-0.5565) H10(-0.5442) H11(-
 0.4586) H15(-0.2781) H16(-0.3166) H17(-0.3892) H18(-0.4193) H22(-0.193) H23(-
 0.1574) H24(-0.0875) H25(-0.0522) H38(-0.2577) H5A(0.0315) H0A(0.1225)
 H2A(0.1628) H3A(0.112) H4AA(0.021) H29(-0.0536) H40(-0.3965) H41(-0.0362) H0B(-
 0.0388) H39(-0.0411) H8A(-0.0441) H7A(-0.0448) H84(-0.3075) H83(-0.3227) H82(-
 0.2495) H81(-0.1599) H80(-0.1454) H72(-0.1716) H78(-0.1541) H77(-0.1786) H76(-
 0.2686) H75(-0.3318) H74(-0.3081) H1B(-0.4006) H66(-0.4257) H67(-0.4282) H68(-
 0.4295) H69(-0.4251) H3B(-0.3297) H70(-0.4253) H58(-0.4075) H2B(-0.3259) H60(-
 0.495) H61(-0.5851) H62(-0.6261) H63(-0.5782) H64(-0.4883) H46(-0.1648) H47(-
 0.2053) H48(-0.2568) H49(-0.2735) H50(-0.2397) H56(-0.1099) H55(-0.0272)
 H54(0.0128) H53(-0.0312) H44(-0.2046) H91A(-0.1717) H91B(-0.1918) H92A(-
 0.1073) H92B(-0.1482) H92C(-0.1168) H87A(-0.2895) H87B(-0.2281) H88A(-0.2419)
 H88B(-0.3056) H88C(-0.2748) H86A(-0.2014) H86B(-0.2616) H85A(-0.1657) H85B(-
 0.1956) H85C(-0.226) H90A(-0.2783) H90B(-0.2606) H89A(-0.3618) H89B(-0.3367)
 H89C(-0.3521)
 Fixed Z: H6(-0.1685) H13B(-0.0833) H4(-0.1596) H1(-0.1647) H52(-0.0992) H2(-
 0.1602) H8(-0.1573) H3(-0.1777) H32(-0.3699) H4A(-0.2035) H36(-0.4378) H33(-
 0.4169) H34(-0.4732) H35(-0.4867) H30(-0.3793) H9(-0.1534) H10(-0.1731) H11(-
 0.1966) H15(-0.2687) H16(-0.3278) H17(-0.3797) H18(-0.3744) H22(-0.2785) H23(-
 0.333) H24(-0.3899) H25(-0.3855) H38(-0.3701) H5A(-0.2085) H0A(-0.1988) H2A(-
 0.1165) H3A(-0.044) H4AA(-0.0537) H29(-0.099) H40(-0.4542) H41(-0.2312) H0B(-
 0.2604) H39(-0.2017) H8A(-0.1138) H7A(-0.0845) H84(-0.1646) H83(-0.2147) H82(-
 0.2467) H81(-0.2278) H80(-0.179) H72(-0.1315) H78(-0.0519) H77(0.0347)
 H76(0.0598) H75(-0.0003) H74(-0.0863) H1B(-0.4603) H66(-0.215) H67(-0.2414)
 H68(-0.1775) H69(-0.0902) H3B(-0.4278) H70(-0.0657) H58(-0.0861) H2B(-0.4063)
 H60(-0.1965) H61(-0.1873) H62(-0.1089) H63(-0.0367) H64(-0.0438) H46(-0.0489)
 H47(0.0085) H48(0.0783) H49(0.0867) H50(0.0289) H56(0.0307) H55(0.0499) H54(-
 0.0014) H53(-0.0793) H44(-0.055) H91A(-0.6024) H91B(-0.6439) H92A(-0.6191)
 H92B(-0.5846) H92C(-0.5594) H87A(-0.562) H87B(-0.5708) H88A(-0.6634) H88B(-
 0.6502) H88C(-0.6419) H86A(-0.5059) H86B(-0.4986) H85A(-0.5177) H85B(-0.4627)
 H85C(-0.5103) H90A(-0.6318) H90B(-0.5839) H89A(-0.5861) H89B(-0.5321) H89C(-
 0.5758)
;