Synthesis of a "Super Bulky" Guanidinate Possessing an Expandable Coordination Pocket.
Maity, Arnab K.; Fortier, Skye; Griego, Leonel; Metta-Magaña, Alejandro J; Inorganic chemistry 53 (2014) 8155–; doi:10.1021/ic501219q

data_4340474
_publ_section_title
;
 Synthesis of a &quot;Super Bulky&quot; Guanidinate Possessing an
 Expandable Coordination Pocket.
;
_journal_issue                   15
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8155
_journal_paper_doi               10.1021/ic501219q
_journal_volume                  53
_journal_year                    2014
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C82 H75 K N3, 2(C6)'
_chemical_formula_sum            'C94 H112 K N3'
_chemical_formula_weight         1322.97
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-04-16
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 100.0920(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.3345(3)
_cell_length_b                   19.1840(4)
_cell_length_c                   15.6017(3)
_cell_measurement_reflns_used    5876
_cell_measurement_temperature    100
_cell_measurement_theta_max      20.37
_cell_measurement_theta_min      2.45
_cell_volume                     3929.31(14)
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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     0.71073
_diffrn_reflns_av_R_equivalents  0.0603
_diffrn_reflns_av_unetI/netI     0.0819
_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       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            47462
_diffrn_reflns_theta_full        24.79
_diffrn_reflns_theta_max         24.79
_diffrn_reflns_theta_min         1.55
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.115
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6604
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0645 before and 0.0501 after correction.
The Ratio of minimum to maximum transmission is 0.8860.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.118
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.621
_refine_diff_density_min         -0.346
_refine_diff_density_rms         0.060
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.04(5)
_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     861
_refine_ls_number_reflns         13389
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.1065
_refine_ls_R_factor_gt           0.0680
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0955P)^2^+1.2050P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1570
_refine_ls_wR_factor_ref         0.1772
_reflns_number_gt                9618
_reflns_number_total             13389
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic501219q_si_004.cif
_cod_data_source_block           Kbulk
_cod_depositor_comments
'Adding full bibliography for 4340472--4340475.cif.'
_cod_original_cell_volume        3929.30(14)
_cod_database_code               4340474
_olex2_refinement_description
;
1. Others
 Fixed Sof: C80M(0.5) C80H(0.25) C80D(0.25) C80E(0.5) C80G(0.25) C80F(0.25)
 Fixed Uiso: H15(0.034) H5A(0.062) H5B(0.062) H5C(0.062) H6A(0.068) H6B(0.068)
 H6C(0.068) H72(0.04) H57(0.026) H70(0.03) H59(0.034) H69(0.036) H49(0.029)
 H68(0.043) H21(0.033) H26(0.041) H39(0.045) H27(0.038) H51(0.031) H36(0.038)
 H66(0.044) H34(0.031) H23(0.041) H13(0.036) H81(0.038) H60(0.038) H38(0.046)
 H45(0.053) H8A(0.057) H8B(0.057) H8C(0.057) H42(0.042) H73(0.046) H80(0.045)
 H44(0.056) H82(0.051) H29(0.055) H76(0.036) H32(0.066) H9A(0.062) H9B(0.062)
 H9C(0.062) H61(0.04) H62(0.039) H63(0.033) H37(0.046) H67(0.044) H78(0.042)
 H4A(0.049) H4B(0.049) H4C(0.049) H79(0.049) H43(0.056) H46(0.044) H31(0.073)
 H40(0.036) H33(0.056) H25(0.045) H30(0.07) H74(0.051) H10A(0.063) H10B(0.063)
 H10C(0.063) H24(0.045) H65(0.036) H75(0.044) H55A(0.145) H55B(0.145)
 H55C(0.145) H54A(0.162) H54B(0.162) H54C(0.162) H56A(0.11) H56B(0.11)
 H56C(0.11)
 Fixed X: H15(0.2158) H5A(0.4289) H5B(0.3112) H5C(0.3445) H6A(0.4) H6B(0.4078)
 H6C(0.4885) H72(0.0266) H57(0.2529) H70(0.2003) H59(0.126) H69(0.2333)
 H49(0.3825) H68(0.3288) H21(0.0228) H26(-0.2788) H39(0.2118) H27(-0.1606)
 H51(0.3401) H36(0.0477) H66(0.4775) H34(0.2811) H23(-0.0701) H13(0.0098)
 H81(0.1645) H60(-0.0453) H38(0.0399) H45(0.5515) H8A(0.442) H8B(0.4511)
 H8C(0.5518) H42(0.2706) H73(-0.1449) H80(0.2389) H44(0.5419) H82(0.3556)
 H29(0.016) H76(0.1025) H32(-0.2576) H9A(0.5766) H9B(0.5125) H9C(0.4586) H61(-
 0.1479) H62(-0.0752) H63(0.0946) H37(-0.042) H67(0.4488) H78(0.3205)
 H4A(0.1905) H4B(0.2251) H4C(0.2294) H79(0.3938) H43(0.4018) H46(0.4165) H31(-
 0.2055) H40(0.3002) H33(-0.1797) H25(-0.2945) H30(-0.0638) H74(-0.1941)
 H10A(0.5428) H10B(0.5667) H10C(0.6279) H24(-0.1876) H65(0.3863) H75(-0.069)
 H55A(0.5805) H55B(0.6041) H55C(0.5475) H54A(0.3975) H54B(0.4658) H54C(0.3523)
 H56A(0.4088) H56B(0.5229) H56C(0.4989)
 Fixed Y: H15(0.303) H5A(0.4586) H5B(0.4382) H5C(0.5185) H6A(0.5741)
 H6B(0.5315) H6C(0.5177) H72(0.5167) H57(0.2211) H70(0.4745) H59(0.2298)
 H69(0.121) H49(0.2207) H68(0.023) H21(0.4572) H26(0.3907) H39(0.0332)
 H27(0.4634) H51(0.4191) H36(0.2166) H66(0.0417) H34(0.2649) H23(0.3057)
 H13(0.4521) H81(0.4972) H60(0.2057) H38(0.0227) H45(0.2971) H8A(0.2775)
 H8B(0.2716) H8C(0.2755) H42(0.1486) H73(0.4969) H80(0.585) H44(0.2021)
 H82(0.6617) H29(0.5756) H76(0.3681) H32(0.5518) H9A(0.3804) H9B(0.4499)
 H9C(0.3839) H61(0.1645) H62(0.1418) H63(0.1685) H37(0.1156) H67(-0.0193)
 H78(0.5625) H4A(0.4657) H4B(0.4924) H4C(0.5442) H79(0.651) H43(0.1277)
 H46(0.3195) H31(0.6609) H40(0.1346) H33(0.4536) H25(0.2737) H30(0.674)
 H74(0.409) H10A(0.3746) H10B(0.4432) H10C(0.3726) H24(0.2321) H65(0.1423)
 H75(0.3455) H55A(0.3268) H55B(0.2763) H55C(0.2466) H54A(0.208) H54B(0.2362)
 H54C(0.2649) H56A(0.3869) H56B(0.3615) H56C(0.4088)
 Fixed Z: H15(0.9989) H5A(0.8823) H5B(0.8741) H5C(0.877) H6A(0.7531)
 H6B(0.6664) H6C(0.7534) H72(0.5048) H57(0.623) H70(0.5273) H59(0.3998)
 H69(0.4232) H49(0.454) H68(0.4051) H21(0.7092) H26(0.5319) H39(0.7392)
 H27(0.6157) H51(0.3717) H36(0.8528) H66(0.6525) H34(0.8007) H23(0.7809)
 H13(0.9273) H81(0.2958) H60(0.3498) H38(0.7487) H45(1.022) H8A(0.6651)
 H8B(0.7685) H8C(0.726) H42(0.9737) H73(0.4528) H80(0.2249) H44(1.1139)
 H82(0.3048) H29(0.7365) H76(0.3447) H32(0.8801) H9A(0.6355) H9B(0.6439)
 H9C(0.5924) H61(0.4465) H62(0.5912) H63(0.6415) H37(0.8065) H67(0.5209)
 H78(0.5253) H4A(0.7456) H4B(0.6581) H4C(0.7391) H79(0.4549) H43(1.0886)
 H46(0.9075) H31(0.8486) H40(0.7828) H33(0.8359) H25(0.5726) H30(0.7783)
 H74(0.3499) H10A(0.8602) H10B(0.8089) H10C(0.7994) H24(0.6991) H65(0.6689)
 H75(0.2941) H55A(0.4353) H55B(0.3597) H55C(0.4343) H54A(0.3143) H54B(0.2469)
 H54C(0.2428) H56A(0.2566) H56B(0.2553) H56C(0.3337)
;