A 30-Membered Nonanuclear Cobalt(II) Macrocycle Containing Phosphonate-Bridged Trinuclear Subunits
Sahoo, Dipankar; Suriyanarayanan, Ramakirushnan; Chandrasekhar, Vadapalli; Crystal Growth & Design 14 (2014) 2725–; doi:10.1021/cg5003594

data_4510583
_publ_section_title
;
 A 30-Membered Nonanuclear Cobalt(II) Macrocycle Containing
 Phosphonate-Bridged Trinuclear Subunits
;
_journal_issue                   6
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              2725
_journal_paper_doi               10.1021/cg5003594
_journal_volume                  14
_journal_year                    2014
_chemical_formula_moiety         '6(C7 H8), C93 H133 Cl9 Co9 N36 O9 P3'
_chemical_formula_sum            'C135 H181 Cl9 Co9 N36 O9 P3'
_chemical_formula_weight         3394.48
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2014-03-12
_audit_creation_method
;
Olex2 1.2
(compiled 2013.11.15 svn.r2834 for OlexSys, GUI svn.r4720)
;
_cell_angle_alpha                69.974(5)
_cell_angle_beta                 83.293(5)
_cell_angle_gamma                64.700(5)
_cell_formula_units_Z            2
_cell_length_a                   18.446(5)
_cell_length_b                   21.371(5)
_cell_length_c                   25.362(5)
_cell_measurement_reflns_used    9951
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      16.33
_cell_measurement_theta_min      2.23
_cell_volume                     8487(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS-2013 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.283
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0385
_diffrn_reflns_av_unetI/netI     0.0527
_diffrn_reflns_Laue_measured_fraction_full 0.283
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            17701
_diffrn_reflns_point_group_measured_fraction_full 0.283
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         16.329
_diffrn_reflns_theta_min         2.067
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.086
_exptl_absorpt_correction_T_max  0.929
_exptl_absorpt_correction_T_min  0.923
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0927 before and 0.0541 after correction.
The Ratio of minimum to maximum transmission is 0.7402.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.328
_exptl_crystal_F_000             3512
_exptl_crystal_size_max          0.074
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.068
_refine_diff_density_max         1.424
_refine_diff_density_min         -0.945
_refine_diff_density_rms         0.156
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.137
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1657
_refine_ls_number_reflns         8698
_refine_ls_number_restraints     933
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.1151
_refine_ls_R_factor_gt           0.1038
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.3000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3158
_refine_ls_wR_factor_ref         0.3387
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7217
_reflns_number_total             8698
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cg5003594_si_001.cif
_cod_data_source_block           4octc
_cod_depositor_comments          'Adding full bibliography for 4510583.cif.'
_cod_database_code               4510583
_shelxl_version_number           2013-3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C2C-C2B
 1.54 with sigma of 0.02
 C8-C21
 1.54 with sigma of 0.02
 C8-C133
 1.39 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C22) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C107) \\sim Ueq, Uanis(C91)
\\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C12) \\sim Ueq:
with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C135) \\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C8)
\\sim Ueq, Uanis(C136) \\sim Ueq, Uanis(C133) \\sim Ueq, Uanis(C21) \\sim Ueq:
with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C118) \\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C1)
\\sim Ueq, Uanis(C300) \\sim Ueq, Uanis(C1B) \\sim Ueq, Uanis(C114) \\sim Ueq:
with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C1K) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C1G)
\\sim Ueq, Uanis(N7) \\sim Ueq, Uanis(N8) \\sim Ueq: with sigma of 0.001 and
sigma for terminal atoms of 0.002
Uanis(C14) \\sim Ueq, Uanis(C1L) \\sim Ueq, Uanis(C1H) \\sim Ueq, Uanis(C1D)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C1F) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(N12) \\sim Ueq, Uanis(C2)
\\sim Ueq, Uanis(C1A) \\sim Ueq: with sigma of 0.001 and sigma for terminal
atoms of 0.002
Uanis(C1J) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(N13) \\sim Ueq, Uanis(N14) \\sim Ueq, Uanis(C93) \\sim Ueq, Uanis(C92)
\\sim Ueq, Uanis(C1N) \\sim Ueq, Uanis(C90) \\sim Ueq, Uanis(C89) \\sim Ueq:
with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(N18) \\sim Ueq, Uanis(N17) \\sim Ueq, Uanis(C83) \\sim Ueq, Uanis(C82)
\\sim Ueq, Uanis(C81) \\sim Ueq, Uanis(C80) \\sim Ueq: with sigma of 0.001 and
sigma for terminal atoms of 0.002
Uanis(C78) \\sim Ueq, Uanis(C77) \\sim Ueq, Uanis(C76) \\sim Ueq, Uanis(C75)
\\sim Ueq, Uanis(C74) \\sim Ueq, Uanis(N20) \\sim Ueq: with sigma of 0.001 and
sigma for terminal atoms of 0.002
Uanis(C84) \\sim Ueq, Uanis(C85) \\sim Ueq, Uanis(C86) \\sim Ueq, Uanis(C87)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O7) \\sim Ueq, Uanis(O9) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C68) \\sim Ueq, Uanis(C67) \\sim Ueq, Uanis(C64) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
Uanis(C53) \\sim Ueq, Uanis(C51) \\sim Ueq, Uanis(N28) \\sim Ueq, Uanis(C49)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C40) \\sim Ueq, Uanis(C84) \\sim Ueq, Uanis(C85) \\sim Ueq, Uanis(C87)
\\sim Ueq, Uanis(C90) \\sim Ueq, Uanis(C92) \\sim Ueq: with sigma of 0.001 and
sigma for terminal atoms of 0.002
Uanis(C82) \\sim Ueq, Uanis(C80) \\sim Ueq, Uanis(C81) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
Uanis(C13) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C28) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
Uanis(N3) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(C32)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(N35) \\sim Ueq, Uanis(N36) \\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C38)
\\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(N33) \\sim Ueq, Uanis(C45) \\sim Ueq,
Uanis(C48) \\sim Ueq, Uanis(C46) \\sim Ueq, Uanis(C59) \\sim Ueq, Uanis(C51)
\\sim Ueq, Uanis(C49) \\sim Ueq, Uanis(N28) \\sim Ueq: with sigma of 0.001 and
sigma for terminal atoms of 0.002
Uanis(C50) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(N27) \\sim Ueq, Uanis(N30) \\sim Ueq, Uanis(N29) \\sim Ueq, Uanis(C55)
\\sim Ueq, Uanis(C56) \\sim Ueq, Uanis(C58) \\sim Ueq: with sigma of 0.001 and
sigma for terminal atoms of 0.002
Uanis(N25) \\sim Ueq, Uanis(N26) \\sim Ueq, Uanis(C61) \\sim Ueq, Uanis(C60)
\\sim Ueq, Uanis(N23) \\sim Ueq: with sigma of 0.001 and sigma for terminal
atoms of 0.002
Uanis(C50) \\sim Ueq, Uanis(N27) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(N26) \\sim Ueq, Uanis(N25) \\sim Ueq, Uanis(C60) \\sim Ueq, Uanis(C61)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C7) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(C57)
\\sim Ueq, Uanis(N21) \\sim Ueq, Uanis(N22) \\sim Ueq, Uanis(C71) \\sim Ueq,
Uanis(C70) \\sim Ueq, Uanis(C73) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C7) \\sim Ueq, Uanis(C23) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C47) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C44) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C7) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C57) \\sim Ueq, Uanis(N21)
\\sim Ueq, Uanis(N22) \\sim Ueq, Uanis(N19) \\sim Ueq, Uanis(C71) \\sim Ueq:
with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C1C) \\sim Ueq, Uanis(C1M) \\sim Ueq, Uanis(C62) \\sim Ueq, Uanis(C42)
\\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C41) \\sim Ueq, Uanis(N31) \\sim Ueq,
Uanis(N32) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(N16) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C15) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
Uanis(N9) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(N9) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C29) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C33) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
Uanis(C10) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C2B) \\sim Ueq, Uanis(C2C) \\sim Ueq, Uanis(C2D) \\sim Ueq, Uanis(C2E)
\\sim Ueq, Uanis(C2F) \\sim Ueq, Uanis(C2G) \\sim Ueq, Uanis(C2H) \\sim Ueq:
with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C1U) \\sim Ueq, Uanis(C1V) \\sim Ueq, Uanis(C1W) \\sim Ueq, Uanis(C1X)
\\sim Ueq, Uanis(C1Y) \\sim Ueq, Uanis(C1Z) \\sim Ueq, Uanis(C2A) \\sim Ueq:
with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C2I) \\sim Ueq, Uanis(C1O) \\sim Ueq, Uanis(C1P) \\sim Ueq, Uanis(C1Q)
\\sim Ueq, Uanis(C1R) \\sim Ueq, Uanis(C1S) \\sim Ueq, Uanis(C1T) \\sim Ueq:
with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C65) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C26) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C3) \\sim Ueq, Uanis(C26) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(N15) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C52) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C35) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(Cl8) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(N10) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C22) = Uanis(C4) = Uanis(C107) = Uanis(C91) = Uanis(C9) = Uanis(C25) =
Uanis(C12)
Uanis(C2E) = Uanis(C2F) = Uanis(C2G) = Uanis(C2H) = Uanis(C2C) = Uanis(C2D)
Uanis(C2B) = Uanis(C2C) = Uanis(C2D) = Uanis(C2E) = Uanis(C2F) = Uanis(C2G) =
Uanis(C2H)
Uanis(C1U) = Uanis(C1V) = Uanis(C1W) = Uanis(C1X) = Uanis(C1Y) = Uanis(C1Z) =
Uanis(C2A)
Uanis(C2I) = Uanis(C1O) = Uanis(C1P) = Uanis(C1Q) = Uanis(C1R) = Uanis(C1S) =
Uanis(C1T)
4.a Riding coordinates:
 N14(H14)
4.b Secondary CH2 refined with riding coordinates:
 C41(H41A,H41B)
4.c Aromatic/amide H refined with riding coordinates:
 C1(H1A), C4(H4), C5(H5), C9(H9), C18(H18), C22(H22), C36(H36A), C66(H66),
 C46(H46), C10(H10), C51(H51), C56(H56), C61(H61), C86(H86), C26(H26), C16(H16),
  C31(H31), C15(H15), C71(H71), C1B(H1B), C91(H91), C81(H81), C107(H107),
 C1H(H1H), C114(H114), C1J(H1J), C76(H76), N12(H12), N1(H1), N36(H36), N24(H24),
  N26(H26A), C135(H135), C133(H133), C1N(H1N), C136(H136), C300(H300), C1P(H1P),
  C1Q(H1Q), C1R(H1R), C1S(H1S), C1T(H1T), C1W(H1W), C1X(H1X), C1Y(H1Y),
 C1Z(H1Z), C2A(H2AA), C2D(H2D), C2E(H2E), C2F(H2F), C2G(H2G), C2H(H2H)
4.d Fitted hexagon refined as free rotating group:
 C1O(C1P,C1Q,C1R,C1S,C1T), C1V(C1W,C1X,C1Y,C1Z,C2A), C2C(C2D,C2E,C2F,C2G,C2H)
4.e Idealised Me refined as rotating group:
 C83(H83A,H83B,H83C), C2(H2A,H2B,H2C), C64(H64A,H64B,H64C), C93(H93A,H93B,
 H93C), C21(H21A,H21B,H21C), C24(H24A,H24B,H24C), C53(H53A,H53B,H53C), C12(H12A,
 H12B,H12C), C84(H84A,H84B,H84C), C17(H17A,H17B,H17C), C49(H49A,H49B,H49C),
 C89(H89A,H89B,H89C), C54(H54A,H54B,H54C), C28(H28A,H28B,H28C), C74(H74A,H74B,
 H74C), C39(H39A,H39B,H39C), C1C(H1CA,H1CB,H1CC), C23(H23A,H23B,H23C), C48(H48A,
 H48B,H48C), C1F(H1FA,H1FB,H1FC), C88(H88A,H88B,H88C), C58(H58A,H58B,H58C),
 C69(H69A,H69B,H69C), C1G(H1GA,H1GB,H1GC), C78(H78A,H78B,H78C), C79(H79A,H79B,
 H79C), C44(H44A,H44B,H44C), C1I(H1IA,H1IB,H1IC), C38(H38A,H38B,H38C), C63(H63A,
 H63B,H63C), C59(H59A,H59B,H59C), C118(H11A,H11B,H11C), C33(H33A,H33B,H33C),
 C1K(H1KA,H1KB,H1KC), C34(H34A,H34B,H34C), C68(H68A,H68B,H68C), C29(H29A,H29B,
 H29C), C1L(H1LA,H1LB,H1LC), C73(H73A,H73B,H73C), C1U(H1UA,H1UB,H1UC), C2B(H2BA,
 H2BB,H2BC), C2I(H2IA,H2IB,H2IC)
;
_shelx_res_checksum              74948
_shelx_hkl_checksum              34523